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.

Examination of a damaged component involves a chain of activities that, first and foremost, requires good observation and documentation. Following receipt and documentation, the features of damage can be recorded and their cause(s) investigated, as this article briefly describes, for typical types of damage experienced for metallic components. This article discusses the processes involved in visual or macroscopic examination of damaged material; the interpretation of fracture features, corrosion, and wear damage features; and the analysis of base material composition. It covers the processes involved in the selection of metallurgical samples, the preparation and examination of metallographic specimens in failure analysis, and the analysis and interpretation of microstructures. Examination and evaluation of polymers and ceramic materials in failure analysis are also briefly discussed.

The characterization, testing, and nondestructive evaluation of ceramics and glasses are vital to manufacturing control, property improvement, failure prevention, and quality assurance. This article provides a broad overview of characterization methods and their relationship to property control, both in the production and use of ceramics and glasses. Important aspects covered include the means for characterizing ceramics and glasses, the corresponding rationale behind them, and relationship of chemistry, phases, and microconstituents to engineering properties. The article also describes the effects that the structure of raw ceramic materials and green products and processing parameters have on the ultimate structure and properties of the processed piece. The effects that trace chemistry and processing parameters have on glass properties are discussed. The article describes mechanical tests and failure analysis techniques used for ceramics.

This article focuses on the visual or macroscopic examination of damaged materials and interpretation of damage and fracture features. Analytical tools available for evaluations of corrosion and wear damage features include energy dispersive spectroscopy, electron probe microanalysis, Auger electron spectroscopy, secondary ion mass spectroscopy, and X-ray powder diffraction. The article discusses the analysis and interpretation of base material composition and microstructures. Preparation and examination of metallographic specimens in failure analysis are also discussed. The article concludes with a review of the evaluation of polymers and ceramic materials in failure analysis.

This article discusses the capabilities and limitations of various material characterization methods that assist in the selection of a proper analytical tool for analyzing particulate materials. Commonly used methods are microanalysis, surface analysis, and bulk analysis. The techniques used for performing microanalysis include scanning electron microscopy and electron probe X-ray microanalysis. The article describes surface analysis techniques, including Auger electron spectroscopy, X-ray photoelectron spectroscopy, and ion-scattering spectroscopy. Bulk analysis techniques, such as X-ray powder diffraction, inductively coupled plasma atomic emission spectroscopy, atomic absorption spectroscopy, and atomic fluorescence spectrometry, are also discussed.

In secondary ion mass spectroscopy (SIMS), an energetic beam of focused ions is directed at the sample surface in a high or ultrahigh vacuum (UHV) environment. The transfer of momentum from the impinging primary ions to the sample surface causes sputtering of surface atoms and molecules. This article focuses on the principles and applications of high sputter rate dynamic SIMS for depth profiling and bulk impurity analysis. It provides information on broad-beam instruments, ion microprobes, and ion microscopes, detailing their system components with illustrations. The article graphically illustrates the SIMS spectra and depth profiles of various materials. The quantitative analysis of ion-implantation profiles, instrumental features required for secondary ion imaging, the analysis of nonmetallic samples, detection sensitivity, and the applications of SIMS are also discussed.

This article describes the sectioning process, some general practices, common tools, and guidelines on how to select a cutting tool for a given metallographic sectioning operation. It provides a discussion on the consumable-abrasive cutting and nonconsumable-abrasive cutting methods for metallographic sectioning. Other methods, including the use of hacksaws, shears, burning torches, wire saws, and electrical discharge machining, are also reviewed. The article reviews the issues related to the specimen test location for certification work as well as process troubleshooting and component failure analysis.

Failure analysis is a process that is performed to determine the causes or factors that have led to an undesired loss of functionality. This article describes some of the factors and conditions that might be considered when approaching a failure analysis problem. It focuses on the key principles, objectives, practices, and procedures of failure analysis. The article provides guidelines on the preparation of a protocol for a failure analysis. It also demonstrates the proper approaches to failure analysis.

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.

Failure analysis is a process that is performed in order to determine the causes or factors that have led to an undesired loss of functionality. This article is intended to demonstrate proper approaches to failure analysis work. The goal of the proper approach is to allow the most useful and relevant information to be obtained. The discussion covers the principles and approaches in failure analysis work, objectives and scopes of failure analysis, the planning stages for failure analysis, the preparation of a protocol for a failure analysis, practices used by failure analysts, and procedures of failure analysis.

Scanning electron microscopy (SEM) has shown various significant improvements since it first became available in 1965. These improvements include enhanced resolution, dependability, ease of operation, and reduction in size and cost. This article provides a detailed account of the instrumentation and principles of SEM, broadly explaining its capabilities in resolution and depth of field imaging. It describes three additional functions of SEM, including the use of channeling patterns to evaluate the crystallographic orientation of micron-sized regions; use of backscattered detectors to reveal grain boundaries on unetched samples and domain boundaries in ferromagnetic alloys; and the use of voltage contrast, electron beam-induced currents, and cathodoluminescence for the characterization and failure analysis of semiconductor devices. The article compares the features of SEM with that of scanning Auger microscopes, and lists the applications and limitations of SEM.

This article focuses on the principles and applications of high-sputter-rate dynamic secondary ion mass spectroscopy (SIMS) for depth profiling and bulk impurity analysis. It begins with an overview of various factors pertinent to sputtering. This is followed by a discussion on the effects of ion implantation and electronic excitation on the charge of the sputtered species. The design and operation of the various instrumental components of SIMS is then reviewed. Details on a depth-profiling analysis of SIMS, the quantitative analysis of SIMS data, and the static mode of operation of time-of-flight SIMS are covered. Instrumental features required for secondary ion imaging are presented and the differences between quadrupole and high-resolution magnetic mass filters are described. The article also reviews the optimum method for analysis of nonmetallic samples and high detection sensitivity of SIMS. It ends with a discussion on a variety of examples of SIMS applications.

Electrogravimetry is a method used to separate and quantify ions of a substance, usually a metal. Quantification of these ions primarily depends on the rate of movement of charged species (ions) in an electric field. This article details the various types of electrometric titrations, namely, conductometric titration, oscillometric (high frequency) titration, potentiometric titration, amperometric titration, biamperometric titration, bipotentiometric titration, and coulometric titration. It also provides a brief outline of the applications of electrometric titrations.

This article endeavors to familiarize the reader with a selection of different ionization designs and instrument components to provide knowledge for sorting the various analytical strategies in the field of solid analysis by mass spectrometry (MS). It begins with a description of the general principles of MS. This is followed by sections providing a basic understanding of instrumentation and discussing the operating requirements as well as practical considerations related to solid sample analysis by MS. Instrumentation discussed include the triple quadrupole mass spectrometer and the time-of-flight mass spectrometer. Inductively coupled plasma and thermal ionization MS provide atomic information, and direct analysis in real-time and matrix-assisted laser-desorption ionization MS are used to analyze molecular compositions. The article describes various factors pertinent to ionization methods, namely glow discharge mass spectrometry and secondary ion mass spectrometry. It concludes with a section on various examples of applications and interpretation of MS for various materials.

Hydrogen damage is a term used to designate a number of processes in metals by which the load-carrying capacity of the metal is reduced due to the presence of hydrogen. This article introduces the general forms of hydrogen damage and provides an overview of the different types of hydrogen damage in all the major commercial alloy systems. It covers the broader topic of hydrogen damage, which can be quite complex and technical in nature. The article focuses on failure analysis where hydrogen embrittlement of a steel component is suspected. It provides practical advice for the failure analysis practitioner or for someone who is contemplating procurement of a cost-effective failure analysis of commodity-grade components suspected of hydrogen embrittlement. Some prevention strategies for design and manufacturing problem-induced hydrogen embrittlement are also provided.

This article focuses on some of the factors pertinent to atomic absorption spectroscopy (AAS). It begins by describing the working principle, critical components, and construction of flame atomic absorption instrumentation. This is followed by sections discussing various types of interferences in AAS, namely vaporization, ionization, matrix interferences, and background correction. Some of the methods for the analysis of microliter-sized samples and methods of standard additions to the sample solution for generating calibration standards are then reviewed. The article concludes with a section on processes involved in matrix matching.

This article provides an overview of the classification of hydrogen damage. Some specific types of the damage are hydrogen embrittlement, hydrogen-induced blistering, cracking from precipitation of internal hydrogen, hydrogen attack, and cracking from hydride formation. The article focuses on the types of hydrogen embrittlement that occur in all the major commercial metal and alloy systems, including stainless steels, nickel-base alloys, aluminum and aluminum alloys, titanium and titanium alloys, copper and copper alloys, and transition and refractory metals. The specific types of hydrogen embrittlement discussed include internal reversible hydrogen embrittlement, hydrogen environment embrittlement, and hydrogen reaction embrittlement. The article describes preservice and early-service fractures of commodity-grade steel components suspected of hydrogen embrittlement. Some prevention strategies for design and manufacturing problem-induced hydrogen embrittlement are also reviewed.

This article describes the principles and applications of Auger electron spectroscopy (AES). It provides information on the instrumentation typically used in the AES, including an electron gun, an electron spectrometer, a secondary electron detector, and an ion gun. The article also describes experimental methods and limitations of the AES, including elemental detection sensitivity, electron beam artifacts, sample charging, spectral peak overlap, high vapor pressure samples, and sputtering artifacts.