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.

A desuperheater diffuser nozzle in the steam supply line failed within nine months of service in an 8.25 MN/sq m (1200 psig) steam line. The nozzle was an austenitic stainless steel casting in conformance to material. The nozzle had numerous cracks on the inside and outside surfaces, and the cracks had penetrated through the wall thickness in several areas. The fracture surfaces had distinct beach markings delineating the crack front, representative of crack propagation stages. The cracks were transgranular and, unlike classical corrosion-fatigue cracks, exhibited branching, characteristic of chloride-induced SCC in austenitic stainless steels. The failure resulted from chloride-induced SCC, possibly assisted by cyclic stress. The recommendation for alternate material for the desuperheater nozzle included nickel base alloys per ASTM B 564, Grades 600 or 800 titanium alloy per ASTM B 367, Grades C3/C4, or ferritic stainless steel alloy per ASTM 182, Grade FXM27.

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 sledge hammer chipped during use. The chip struck a by stander in the eye, leading to its loss. The hammerhead surface was examined visually, nondestructively (magnetic particle method), and stereo microscopically, and a microstructural analysis of a cross section of the head was conducted using optical microscope. Chemical composition of the hammerhead was determined by emission spectrometry. The chemical compositions of the chip and hammer head were compared using energy-dispersive analysis. Microhardness versus distance from the striking face was also determined. The hammerhead material was UNS G10800 (AISI/SAE grade 1080). Excessive hardnesses were measured in the first 3 mm (0. 12 in.) below the striking surface, indicating that there was lack of control during the final tempering operation.

Radiant tubes that failed prematurely in an ethylene cracking furnace were analyzed to determine the cause of their early demise. The tubes were made from austenitic heat-resistant steel and cracked along their longitudinal axis. New and used tubes were compared using scanning electron microscopy, energy dispersive x-ray spectrometry, and mechanical property testing. This provided critical information and revealed that improper coking and decoking had removed the protective oxide layer (Cr 2 O 3 ) that normally prevents coke deposits from forming on exposed surfaces. Without this layer, coke readily accumulates on the surface of the tubes, fueling carbon diffusion into the metal and a corresponding degradation in microstructure and loss of ductility at high temperatures.

A back wall riser tube in a high pressure boiler failed, interrupting operations in a cogeneration plant. The failure occurred in a tube facing the furnace, causing eight ruptured openings over a 1.8 m section. The investigation consisted of an on-site visual inspection, nondestructive testing, energy dispersive x-ray analysis, and inductively coupled plasma mass spectrometry. The tube was made from SA 210A1 carbon steel that had been compromised by wall thinning and the accumulation of fire and water-side scale deposits. Investigators determined that the tube failed due to prolonged caustic attack that led to ruptures in areas of high stress. The escaping steam eroded the outer surface of the tube causing heavy loss of metal around the rupture points.

Several stainless steel coils cracked during a routine unwinding procedure, prompting an investigation to determine the cause. The analysis included optical and scanning electron microscopy, energy-dispersive x-ray spectrometry, and tensile testing. An examination of the fracture surfaces revealed a brittle intercrystalline mode of fracture with typical manifestations of clear grain facets. Branched and discrete stepwise microcracks were also found along with unusually high levels of residual hydrogen. Mechanical tests revealed a marked loss of tensile ductility in the defective steel with elongations barely approaching 8%, compared to 50% at the time of delivery weeks earlier. Based on the timing interval and the fact that failure occurred at operating stresses well below the yield point of the material, the failure is being attributed to hydrogen-induced damage. Potential sources of hydrogen are considered as are remedial measures for controlling hydrogen content in steels.

Linear indications on the outer surface of a cross in a piping system were revealed by dye-penetrant examination. The cross was specified to be SA403 type WP 304 stainless steel. The cross had been subjected to induction-heating stress improvement. The linear indications on the cross were located in wide bands running circumferentially below the cross-to-cap weld and above the cap-to-discharge-pipe weld. The material was found to conform to the requirements both in terms of hardness and strength. Intergranular cracks filled with oxide were observed on metallographic analysis of a sectioned and oxalic acid etched sample. The grain size was found to exceed the ASTM standard. No indications of sensitization were observed during testing with practice A of ASTM A 262. Definitive evidence of contaminants to support SCC as the failure mechanism was not disclosed during analysis. It was concluded that overheating or burning of the forging, which classically results in large grain size, intergranular fractures, and fine oxide particles dispersed throughout the grains was the possible reason for the failure.

Field metallography and replication were performed on a type 316 stainless steel column in diglycol amine vacuum service to determine the cause of visible OD pitting on the column in several areas above the insulation support rings. The examination revealed transgranular stress-corrosion cracking beneath the pitted areas on the OD. The likely cause of the cracking was chloride stress corrosion, with chlorides deriving from the marine atmosphere and concentrating under the insulation around the support rings. A complete insulation evaluation, including repair or replacement, was recommended to prevent chloride buildup. Painting of the steel surface with an epoxy-phenolic or epoxy-coal tar was also suggested.

A 5000-gal (20,000-L) hot-water holding tank fractured at a large automotive manufacturing plant. The tank was made from Type 304 austenitic stainless steel. The inner diameter of the tank displayed a macroscopic, web-like network of cracks that deceptively suggested intergranular stress-corrosion cracking. The problem, however, originated on the outside surface of the tank where a tensile stress (due to low applied stress and fabrication-induced residual stresses) accelerated the growth of numerous stress corrosion cracks that eventually broke through to the inner surface, causing leakage and ultimately failure.

The presence of subsurface cracks in a longitudinal weld seam of an AISI type 316 stainless steel heat-exchanger shell was revealed by radiographic testing. Numerous intergranular cracks associated with the root pass of the weld, which had propagated both parallel and normal to the weld seam, were revealed by metallographic examination (hot shortness). It was indicated by energy-dispersive spectroscopy that type 316 electrode was not used for the root pass and instead a nickel-copper alloy electrode was employed. It was thus concluded that cracking was caused due to the use of an incorrect electrode for the root pass as these electrodes are crack sensitive if overheated. The weld seam was completely ground out and replaced with the correct electrode material as a corrective measure.

An aluminum brass seawater surface condenser failed due to pitting after less than one year of service. Large pits filled with a green deposit were evidenced under the nonuniform black scale present over the entire inside surface of the tube. The black deposit was identified as primarily copper sulfide, with zinc and aluminum sulfides while the green deposit was revealed to be copper chloride. The combination of sulfide and chloride attack on the tubes was concluded to have resulted in the failure. Injection of ferrous sulfate upstream of the condenser which could aid the formation of protective oxide films was recommended.

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.

This article provides information on the chemical characterization of surfaces by Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy (XPS), and time-of-flight secondary ion mass spectrometry (TOF-SIMS). It describes the basic theory behind each of these techniques, the types of data produced from each, and some typical applications. The article explains the strengths of AES, XPS, and TOF-SIMS based on data obtained from the surface of a slightly corroded stainless steel sheet.

The case study presented in this article details the failure investigation of an M50 alloy steel bearing used in a jet engine gearbox drive assembly. It discusses the investigative steps and analytic tools used to determine the root cause, highlighting the importance of continuous, thorough questioning by the investigating activity. The combined analyses demonstrated that the bearing failed by a single event overload as evidenced by bulk deformation and traces of foreign material on the rolling elements. The anomalous transferred metal found on the rolling elements subsequently led to the discovery of overlooked debris in an engine chip detector, and thus resulted in a review of several maintenance practices.

This article covers the three most popular techniques used to characterize the very outermost layers of solid surfaces: Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy (XPS), and time-of-flight secondary ion mass spectrometry (TOF-SIMS). Some of the more important attributes are listed for preliminary insight into the strengths and limitations of these techniques for chemical characterization of surfaces. The article describes the basic theory behind each of the different techniques, the types of data produced from each, and some typical applications. Also discussed are the different types of samples that can be analyzed and the special sample-handling procedures that must be implemented when preparing to do failure analysis using these surface-sensitive techniques. Data obtained from different material defects are presented for each of the techniques. The examples presented highlight the typical data sets and strengths of each technique.

Pendant-style reheater, constructed of ASME SA-213, grade T-11, steel ruptured. A set of four tubes, specified to be 64 mm OD x 3.4 mm minimum wall thickness was examined. A small quantity of loose debris was removed from the inside of one of the tubes. The major constituent was revealed by EDS analysis of the debris to be iron with traces of phosphorus, manganese, sodium, calcium, copper, zinc, potassium, silicon, chromium, and molybdenum. Thus the debris was interpreted to be the scale from ID of the tube with boiler feedwater chemicals from the attemperation spray. The likely cause of failure was concluded to be exfoliation of the scale from the ID surface of the tube. Creep failures were interpreted to be caused by localized temperatures higher than the maximum service temperature. Replacement of the affected tubes was recommended. Inspection of the tubes by radiography to find the circuits with the greatest accumulation of debris and replacing them as necessary was recommended on an annual basis.

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.

This article is a compilation of abbreviations of terms, techniques, standards, compounds, and properties of materials that are relevant to the characterization and failure analysis of plastics.