This article discusses fractures and cracks due to ancient artifact weaknesses. It provides several case studies to aid the appreciation of fractography as a diagnostic technique and to understand the importance of cracking. These case histories concern ancient gold and silver alloys, bronzes, and wrought irons. The article considers the applicabilities of fractography, metallography, and chemical analyses in answering archaeological and archaeometallurgical questions. The article also discusses the restoration and conservation of corroded and embrittled artifacts, including the use of coatings.

This article addresses some established protocols for characterizing thermoplastics and whether they are homogeneous resins, alloyed, or blended compositions or highly modified thermoplastic composites. It begins with a discussion on characterizing mechanical, rheological, and thermal properties of polymer. This is followed by a section describing molecular weight determination using viscosity measurements. Next, the article discusses the use of cone and plate and parallel plate geometries in melt rheology. It then reviews the processes involved in the analysis of thermoplastic resins by chromatography. Finally, the article covers three operations of thermoanalysis, namely differential scanning calorimetry, thermogravimetric analysis, and thermomechanical testing.

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.

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.

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.

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 is a detailed account of optical emission spectroscopy (OES) for elemental analysis. It begins with a discussion on the historical background of OES and development trends in OES methods. This is followed by a description of the general principles and optical systems of OES, along with various types of emission sources commonly used for OES. Some of the processes involved in calibration and quantification of OES for direct solids analysis by the ratio method are then described. The article ends with a discussion on the applications of each type of emission sources.

This article provides a detailed account of the basic concepts of Rutherford backscattering spectrometry (RBS). It begins with a description of the principles of RBS, as well as the effect of channeling in conjunction with backscattering measurements and the effect of energy loss under this condition. This is followed by a section on equipment used in RBS analysis. Channel-energy conversion, energy-depth conversion, and separation of the dechanneling background are then discussed as the main steps of RBS data analysis. The article also discusses the applications of RBS—including composition of bulk samples, thin-film composition and layer thickness, impurity profiles, damage depth profile, and surface peak—as well as the various codes developed to simulate it.

This article presents a summary of the chemical fundamentals, general techniques, limitations, and applications of chemical spot testing as well as a brief overview of innovations and specialized applications. A list of selected reagents, including abbreviated instructions for preparing the reagent solution(s), for performing the spot test, and for interpreting the results, is also included. The article discusses two specialized applications of qualitative analysis, namely illicit drug identification and spacecraft drinking water quality testing. It also contains tables listing common presumptive tests for detecting anions and cations in aqueous solution.

This article focuses on wet chemical methods that have stood the test of time in laboratories around the world. It begins with a description of the appropriateness of classical wet methods. This is followed by sections on sampling procedures, basic chemical equilibria, and wet analytical chemistry. Mechanical methods and nonoxidizing acids and/or acid mixtures for dissolving solid samples for wet chemical analysis are then reviewed. Qualitative methods that are used to identify materials by wet chemical reaction are also included. The article provides information on various methods for the separation of chemical mixtures and on the types of gravimetry and titrimetry. Strategies for removing inclusions are also included to aid in their compositional understanding. The article also briefly describes the processes involved in chemical surface studies and partitioning of oxidation states. It ends by presenting some examples of the applications of classical wet methods.

This article is dedicated to gas chromatography (GC), covering the chromatographic method and primary components of a modern GC apparatus. The components include the carrier gas cylinder, flow controller and pressure regulator, sample inlet and injection port, column oven, and detector. Common GC detectors are the thermal conductivity cell detector, flame ionization detector, electron capture detector, sulfur chemiluminescence detector, and nitrogen-phosphorus detector.

This article briefly describes the capabilities of gas chromatography/mass spectrometry, which is used to qualitatively and quantitatively determine organic (and some inorganic) compound purity and stability and to identify components in a mixture. The discussion covers in more detail gas chromatography/mass spectrometry (GC/MS) instrumentation, interpreting mass spectra, GC/MS methodology, and GC/MS advances. Sample preparation, which is very important in GC/MS to avoid erroneous data and to minimize maintenance and troubleshooting of the instrument, is also discussed. Further, the article highlights the state of the art in the MS detector technology.

This article describes high-performance liquid chromatography and ultra-high-performance liquid chromatography that are used to separate and quantify the chemical components in any sample that can be dissolved in a liquid. This includes pharmaceutical drugs, medicinal plant extracts, food constituents, flavors, fragrances, industrial chemicals, pesticides, and pollutants. Readers are introduced to the most commonly employed mode, reverse-phase chromatography, with examples and an exclusive focus on commercially available instruments and consumables. The discussion covers the various processes involved in liquid chromatography, including assessing a separation of sample components, adjusting the mobile phase, choosing the stationary phase, optimizing a separation, preparing real samples, and analyzing complex samples.

This article presents a detailed account of ion chromatography (IC). It begins by describing the principles of common separation modes in IC. This is followed by a section on the different modes of detection, namely suppressed conductivity detection, nonsuppressed conductivity detection, spectrophotometric detection, and electrochemical detection. Various separation modes in IC are then described. The article further provides information on various eluents species, analyte range, and sample preparation techniques in IC. It ends by providing information on the instrumentation and applications and future directions of IC.

This article describes various methods of electrochemical analysis, namely coulometry, electrogravimetry, voltammetry, electrometric titration, and nanometer electrochemistry. The discussion covers the general uses, sample requirements, application examples, advantages, and limitations of these methods. Some of the factors pertinent to electrochemical cells are also provided. In addition, the article provides information on various potentiometric membrane electrodes used to quantify numerous ionic and nonionic species.

This article provides a detailed account of the concepts and applications of neutron activation analysis (NAA), covering the basic principles and neutron reactions of NAA as well as calibration methods used for NAA. The discussion also covers the factors pertinent to analytical sensitivity achievable with NAA, common neutron sources, sample-handling technique, and automated systems of NAA. The categories of NAA covered are instrumental neutron activation analysis, epithermal neutron activation analysis, radiochemical neutron activation analysis, 14 MeV fast neutron activation analysis, delayed neutron activation analysis, and prompt gamma activation analysis.

This article is a detailed account of the principles of electron-excited X-ray microanalysis. It begins by discussing the physical basis of electron-excited X-ray microanalysis and the advantages and limitations of energy dispersive spectrometry (EDS) and wavelength dispersive spectrometry for electron probe microanalysis. Key concepts for performing qualitative analysis and quantitative analysis by electron-excited X-ray spectrometry are then presented. Several sources that lead to measurement uncertainties in the k-ratio/matrix corrections protocol are provided, along with the significance of the raw analytical total. Sections on accuracy of the standards-based k-ratio/matrix corrections protocol with EDS and processes of analysis when severe peak overlap occurs are also included. The article provides information on low-atomic-number elements, iterative qualitative-quantitative analysis for complex compositions, and significance of standardless analysis in the EDS software. It ends with a section on the processes involved in elemental mapping for major and minor constituents.

This article focuses on the principles and applications of X-ray photoelectron spectroscopy (XPS) for the analysis of elemental and chemical composition. The discussion covers the nomenclature, instruments, and specimen preparation process of XPS. Some of the factors pertinent to the calibration of materials for accurate measurements using XPS are provided, along with some aspects of the accuracy in quantitative analysis by XPS. In addition, the article presents examples of how XPS data can be used to solve problems with surface interactions.