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.

The purpose of this investigation was to determine the cause of the ultrasonic signal attenuation noted during an inspection of a composite aircraft component. Although ultrasonics was able to identify the location of the defective areas, destructive analysis had to be utilized to determine the exact nature of the defect. The investigation describes how cross-sectioning, fractography, and chemical analysis were utilized to determine the type of defect responsible for the signal attenuation.

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.

This article reviews the abrasive and adhesive wear failure of several types of reinforced polymers, including particulate-reinforced polymers, short-fiber reinforced polymers (SFRP), continuous unidirectional fiber reinforced polymers (FRP), particulate-filled composites, mixed composites (SFRP and particulate-filled), unidirectional FRP composites, and fabric reinforced composites. Friction and wear performance of the composites, correlation of performance with various materials properties, and studies on wear-of failure mechanisms by scanning electron microscopy are discussed for each of these types.

Failure analysis results were employed to identify a better alloy. Chipper knives used in the field to chip logs failed frequently. The knives were made of alloys with a composition of Fe-0.48C-0.30Mn-0.90Si-8.50Cr-1.35Mo-1.20W-0.30V. The development of tougher alloy steel with superior properties was initiated. The nominal composition of Fe-0.50C-0.30Mn-0.40Si-5.00Cr-2.00Mo was developed which achieved the goals of edge retention, resistance to softening under frictional heating, wear resistance, ease of heat treatment, dimensional stability in heat treatment, grindability, and low alloy cost. A chip harvester made from this composition was tested in field with older composition knives. It was found that the new knives outperformed the older knives. The key to the development was interpreted to be careful study of a number of failed knives with different problems used in different types of operations.

This article describes some of the common elemental composition analysis methods and explains the concept of referee and economy test methods in failure analysis. It discusses different types of microchemical analyses, including backscattered electron imaging, energy-dispersive spectrometry, and wavelength-dispersive spectrometry. The article concludes with information on specimen handling.

An electron probe microanalyzer was applied to the study of service failures (due to severe heating) of aluminum wire connections in residential electrical circuits. Perturbed regions in which the composition underwent a change during the failure were revealed by optical and scanning electron microscopy of the contacts. A sequence of iron-aluminum compositions that shift from the pure aluminum of the wire to the nearly pure iron of the screw was revealed by analyses of two distinct layers formed on the aluminum/iron region. The compositions were found to correspond to specific intermetallic compounds found in the aluminum-iron phase diagram. Similar compositional variations were noted at the aluminum/brass interface. It was concluded that the failure of the electrical junction due to extreme heating was related to the formation of intermetallic compounds at the current carrying interfaces. These intermetallics were established to have a high resistance causing significant resistive heating.

Creep crack growth and fracture toughness tests were performed using test material machined from a seam welded ASTM A-155-66 class 1 (2.25Cr-1Mo) steel steam pipe that had been in service for 15 years. The fracture morphology was examined using SEM fractography. Dimpled fracture was found to be characteristic of fracture toughness specimens. Creep crack growth generally followed the fusion line region and was characterized as dimpled fracture mixed with cavities. These fracture morphologies were similar to those of an actual steam pipe. It was concluded that creep crack growth behavior was the prime failure mechanism of seam-welded steam pipes.

Hardenability evaluation is typically applied to heat treatment process control, but can also augment standard metallurgical failure analysis techniques for steel components. A comprehensive understanding of steel hardenability is an essential complement to the skills of the metallurgical failure analyst. The empirical information supplied by hardenability analysis can provide additional processing and service insight to the investigator. The intent of this paper is to describe some applications of steel thermal response concepts in failure analysis, and several case studies are included to illustrate these applications.

Cast iron bearing caps in tractor engines fractured repeatedly after only short operating periods. The fracture originated in a cast-in groove and ran approximately radially to the shaft axis. The smallest cross section was at the point of fracture. The core structure of the caps consisted of graphite in pearlitic-ferritic matrix. Casting stresses did not play a decisive role because of the simple shape of the pieces that were without substantial cross sectional variations. Two factors exerted an unfavorable effect in addition to comparatively low strength. First, the operating stress was raised locally by the sharp-edged groove, and second, the fracture resistance of the cast iron was lowered at this critical point by the existence of a ferritic bright border. To avoid such damage in the future it was recommended to observe one or more of the following precautions: 1) Eliminate the grooves; 2) Remove the ferritic bright border; 3) Avoid undercooling in the mold and therefore the formation of granular graphite; 4) Inoculate with finely powdered ferrosilicon into the melt for the same purpose; and, 5) Anneal at lower temperature or eliminate subsequent treatment in consideration of the uncomplicated shape of the castings.

An investigation was conducted to better understand the time-dependent degradation of thermal barrier coated superalloy components in gas turbines. First-stage vanes are normally subjected to the highest gas velocities and temperatures during operation, and were thus the focus of the study. The samples that were analyzed had been operating at 1350 °C in a gas turbine at a combined-cycle generating plant. They were regenerated once, then used for different lengths of time. The investigation included chemical analysis, scanning electron microscopy, SEM/energy dispersive spectroscopy, and x-ray diffraction. It was shown that degradation is driven by chemical and mechanical differences, oxide growth, depletion, and recrystallization, the combined effect of which results in exfoliation, spallation, and mechanical thinning.

An air blower in an electric power plant failed unexpectedly when a roller bearing in the drive motor fractured along its outer ring. Both rings, as well as the 18 rolling elements, were made from GCr15 bearing steel. The bearing also included a machined brass (MA/C3) cage and was packed with molybdenum disulfide (MoS 2 ) lithium grease. Metallurgical structures and chemical compositions of the bearing’s matrix materials were inspected using a microscope and photoelectric direct reading spectrometer. SEM/EDS was used to examine the local morphology and composition of fracture and contact surfaces. Chemical and thermal properties of the bearing grease were also examined. The investigation revealed that the failure was caused by wear due to dry friction and impact, both of which worsened as a result of high-temperature degradation of the bearing grease. Fatigue cracks initiated in the corners of the outer ring and grew large enough for a fracture to occur.

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.

Wet natural gas was dried by being passed through a carbon steel vessel that contained a molecular-sieve drying agent. The drying agent became saturated after several hours in service and was regenerated by a gas that was heated to 290 to 345 deg C in a salt-bath heat exchanger. The tee joint in the piping between the heat exchanger and the sieve bed failed after 12 months. A hole in the tee fitting and a corrosion product on the inner surface of the pitting was revealed by visual examination. Iron sulfide was revealed by chemical analysis of the scale which indicated hydrogen sulfide attack on the carbon steel. The presence of oxygen was indicated by the carbon and sulfur found in the scale on the piping and in the sieves indicated that oxygen combined with moisture produced conditions for attack of hydrogen sulfide on carbon steel. Turbulence with some effect from the coarse grain size was interpreted to have contributed. The piping material was changed from carbon steel to AISI type 316 stainless steel as it is readily weldable and resistant to corrosion by hydrogen sulfide.

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 bent Ni-Cu Monel 400 alloy tube, which operated as part of a pipeline in a petrochemical distillery, failed by through-thickness cracking. The pipeline was used to carry a stream of gaseous hydrocarbons containing hydrochloric acid (HCl) into a reaction tower. The tower provided a caustic solution (NaOH) to remove HCl from the stream, before the latter was directed to a burner. Metallographic examination showed that the cracks were intergranular and were frequently branched. Although nominal chemical composition of the component was found within the specified range, energy dispersive x-ray analysis (EDXA) indicated significant segregation of sulfur and chlorine along the grain boundaries. Failure was attributed to hypochlorous-acid (HClO)-induced stress-corrosion cracking (SCC). The HClO was formed by the reaction of HCl with atmospheric O 2 that entered the tube during shutdowns and startups. Residual stresses, originating from in situ bend forming of the tube during assembly of the line, provided a driving force for crack growth, and the segregation of sulfur on grain boundaries made the material more susceptible to cracking.

Failure analysis was performed on a fractured impeller from a boiler feed pump of a fossil fuel power plant. The impeller was a 12% Cr martensitic stainless steel casting. The failure occurred near the outside diameter of the shroud in the vicinity of a section change at the shroud/vane junction. Sections cut from the impeller were examined visually and by SEM fractography. Microstructural, chemical, and surface analyses and surface hardness tests were conducted on the impeller segments. The results indicated that the impeller failed in fatigue with casting defects increasing stress and initiating fracture. In addition, the composition and hardness of the impeller did not meet specifications. Revision of the casting process and institution of quality assurance methods were recommended.

Door-closer cylinder castings manufactured of class 30 gray iron were breaking during machining. The manufacturing source reported that a random sampling of castings from this lot had hardnesses from 180 to 210 HRB. Based on the color of the components, heat treatment of these castings was suspected. Metallurgical examination on two representative castings supported the conclusions that the cracks in these gray iron door closers that were present either before or during the heat treatment were attributed to a substandard microstructure of the wrong type of graphite combined with excessive ferrite. This anomalous structure is caused by shortcomings in the foundry practice of chemical composition, solidification, and inoculation control. Judging from the microstructure, the strength of the material was lower than desired for class 30 gray iron, and the suspected heat treatment further reduced the strength. Recommendations included that the chemistry and inoculation should be controlled to produce type A graphite structure. The chemistry control should aim for a carbon equivalent close to 4.3% to achieve adequate fluidity for thin sections and to alleviate gas defects.

Rotor blades in the compressor section of a J79 engine had failed. Optical, stereoscopic, microhardness testing, and SEM examinations were conducted to determine the cause. The blades were made of STS403 and were used uncoated. They were damaged over an extensive area, from the 15th through the 17th compressor stages, as were stator vanes and casing sections. The fractured surface of the 17th blade showed multiple origins along with secondary cracking and extensive propagation that preceded separation. The metallographic analysis of the microstructure suggested work hardening. Based on the results, the cause of the fractured blade was high-amplitude fatigue due to severe stall. After normal engine usage of five months, the blade fractured sending fragments throughout the combustion and turbine sections.

An experimental high-temperature rotary valve was found stuck due to growth and distortion after approximately 100 h. Gas temperatures were suspected to have been high due to overfueled conditions. Both the rotor and housing in which it was stuck were annealed ferritic ductile iron similar to ASTM A395. Visual examination of the rotor revealed unusually heavy oxidation and thermal fatigue cracking along the edge of the gas passage. Material properties, including microstructure, composition, and hardness, of both the rotor and housing were evaluated to determine the cause of failure. The microstructure of the rotor was examined in three regions. The shaft material, the heavy section next to the gas passage and the thin edge of the rotor adjacent to the gas passage. The excessive gas temperatures were responsible for the expansion and distortion that prevented rotation of the rotor. Actual operating temperatures exceeded those intended for this application. The presence of transformation products in the brake-rotor edge indicated that the lower critical temperature had been exceeded during operation.