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.

New type 321 corrosion-resistant steel heat shields were cracking during welding operations. A failure analysis was performed. The cause was found to be chloride induced stress-corrosion cracking. Packaging was suspected and confirmed to be the cause of the chloride contamination. A contributing factor was the length of time spent in the packaging, 21 years.

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.

The causes of cracking of an as-drawn 90-10 cupronickel tube during mechanical working were investigated to determine the source of embrittlement. Embrittlement was sporadic, but when present was typically noted after the first process anneal. Microstructural and chemical analyses were performed on an embrittled section and on a section from a different lot that did not crack during forming. The failed section showed an intergranular fracture path. Examination of the fracture surfaces revealed the presence of tellurium at the grain boundaries. The source of the tellurium was thought to be contamination occurring in the casting process that became concentrated in the recycled skimmings. It was recommended that future material specifications for skimmings and for externally obtained scrap copper include a trace analysis for tellurium.

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.

High-level radioactive wastes generated during the processing of nuclear materials are kept in large underground storage tanks made of low-carbon steel. The wastes consist primarily of concentrated solutions of sodium nitrate and sodium hydroxide. Each of the tanks is equipped with a purge ventilation system designed to continuously remove hydrogen gas and vapors without letting radionuclides escape. Several intergranular cracks were discovered in the vent pipe of one such system. The pipe, made of galvanized steel sheet, connects to an exhaust fan downstream of high-efficiency particulate air filters. The failure analysis investigation concluded that nitrate-induced stress-corrosion cracking was the cause of the failure.

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.

The scanning electron microscope (SEM) is one of the most versatile instruments for investigating the microscopic features of most solid materials. The SEM provides the user with an unparalleled ability to observe and quantify the surface of a sample. This article discusses the development of SEM technology and operating principles of basic systems of SEM. The basic systems covered include the electron optical column, signal detection and display equipment, and the vacuum system. The processes involved in the preparation of samples for observation using an SEM are described, and the application of SEM in fractography is discussed. The article covers the failure mechanisms of ductile failure, brittle failure, mixed-mode failure, and fatigue failure. Lastly, image dependence on microscope type and operating parameters is also discussed.

The US Army Research Laboratory performed a failure investigation on a broken main landing gear mount from an AH-64 Apache attack helicopter. A component had failed in flight, and initially prevented the helicopter from safely landing. In order to avoid a catastrophe, the pilot had to perform a low hover maneuver to the maintenance facility, where ground crews assembled concrete blocks at the appropriate height to allow the aircraft to safely touch down. The failed part was fabricated from maraging 300 grade steel (2,068 MPa [300 ksi] ultimate tensile strength), and was subjected to visual inspection/light optical microscopy, metallography, electron microscopy, energy dispersive spectroscopy, chemical analysis, and mechanical testing. It was observed that the vacuum cadmium coating adjacent to the fracture plane had worn off and corroded in service, thus allowing pitting corrosion to occur. The failure was hydrogen-assisted and was attributed to stress corrosion cracking (SCC) and/or corrosion fatigue (CF). Contributing to the failure was the fact that the material grain size was approximately double the required size, most likely caused from higher than nominal temperatures during thermal treatment. These large grains offered less resistance to fatigue and SCC. In addition, evidence of titanium-carbo-nitrides was detected at the grain boundaries of this material that was prohibited according to the governing specification. This phase is formed at higher thermal treatment temperatures (consistent with the large grains) and tends to embrittle the alloy. It is possible that this phase may have contributed to the intergranular attack. Recommendations were offered with respect to the use of a dry film lubricant over the cadmium coated region, and the possibility of choosing an alternative material with a lower notch sensitivity. In addition, the temperature at which this alloy is treated must be monitored to prevent coarse grain growth. As a result of this investigation and in an effort to eliminate future failures, ARL assisted in developing a cadmium brush plating procedure, and qualified two Army maintenance facilities for field repair of these components.

Corrosion is the deterioration of a material by a reaction of that material with its environment. The realization that corrosion control can be profitable has been acknowledged repeatedly by industry, typically following costly business interruptions. This article describes the electrochemical nature of corrosion and provides the typical analysis of environmental- and corrosion-related failures. It presents common methods of testing of laboratory corrosion and discusses the processes involved in the prevention of environmental- and corrosion-related failures of metals and nonmetals.

The purpose of this investigation was to determine the root cause of the differences noted in the fatigue test data of main rotor spindle assembly retaining rods fabricated from three different vendors, as part of a Second Source evaluation process. ARL performed dimensional verification, accessed overall workmanship, and measured the respective surface roughness of the rods in an effort to identify any discrepancies. Next, mechanical testing was performed, followed by optical and electron microscopy, and chemical analysis. Finally, ARL performed laboratory heat treatments at the required aging temperature and follow-up mechanical testing.

While there are many fracture mechanisms that can lead to the failure of a plastic component, environmental stress cracking (ESC) is recognized as one of the leading causes of plastic failure. This article focuses on unpacking the basic concepts of ESC to provide the engineer with a better understanding of how to evaluate and prevent it. It then presents factors that affect and contribute to the susceptibility of plastic to ESC: material factors, chemical factors, stress, and environmental factors. The article includes the collection of background information to understand the circumstances surrounding the failure, a fractographic evaluation to assess the cracking, and analytical testing to evaluate the material, design, manufacturing, and environmental factors.

This article discusses pressure vessels, piping, and associated pressure-boundary items of the types used in nuclear and conventional power plants, refineries, and chemical-processing plants. It begins by explaining the necessity of conducting a failure analysis, followed by the objectives of a failure analysis. Then, the article discusses the processes involved in failure analysis, including codes and standards. Next, fabrication flaws that can develop into failures of in-service pressure vessels and piping are covered. This is followed by sections discussing in-service mechanical and metallurgical failures, environment-assisted cracking failures, and other damage mechanisms that induce cracking failures. Finally, the article provides information on inspection practices.