This article provides a brief account of glow discharge mass spectrometry (GDMS) for direct determination of trace elements in solid samples and for fast depth profiling in a great variety of innovative materials. It begins by describing the general principles of GDMS. This is followed by a discussion on the various components of a GDMS system as well as commercial GDMS instruments. A description of processes involved in specimen preparation and cleaning in GDMS is then presented. Various problems pertinent to multielemental calibrations in GDMS are discussed along with measures to overcome them. The article further provides information on the processes involved in the analytical setup of parameters in GDMS, covering the steps involved in the analysis of GDMS data. It ends with a section on the application and interpretation of GDMS in the metals industry.

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.

This article discusses the basic principles of inductively coupled plasma mass spectrometry (ICP-MS), covering different instruments used for performing ICP-MS analysis. The instruments covered include the sample-introduction system, ICP ion source, mass analyzer, and ion detector. Emphasis is placed on ICP-MS applications in the semiconductor, photovoltaic, materials science, and other electronics and high-technology areas.

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 is an overview of the division Surface Analysis of this volume. The division covers various developed surface-analysis techniques, such as scanning probe and atomic force microscopy. The division focuses on the analysis of surface layers that are less than 100 nm. A quick reference summary of surface-analysis methods is presented in this article.

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.

Spark source mass spectrometry (SSMS) is an analytical technique used for determining the concentration of elements in a wide range of solid samples, including metals, semiconductors, ceramics, geological and biological materials, and air and water pollution samples. This article discusses the basic principles of spark source technique; SSMS instrumentation such as ion source, electric sector, and magnetic sector; sample preparation; and test procedures of SSMS. Some of the related techniques to SSMS are laser ionization mass spectrometry and laser-induced resonance ionization mass spectrometry. The ions produced in SSMS are detected by either the photometric method or electrical detection method and quantitatively measured by techniques such as internal standardization techniques, isotope dilution, multi element isotope dilution, and dry spike isotope dilution. The detected spark source spectrum contains all the elemental data of the tested sample. Finally, the article exemplifies the applications of SSMS.

Quality control of cemented carbides includes the evaluation of physical and chemical properties of constituent raw material powders, powder blends/formulations, green compacts, and fully dense finished product. This article provides a summary of the underlying principles and size ranges for the American Society for Testing and Materials (ASTM) standard methods of particle sizing and distribution. It presents the methods used to analyze the chemical composition of cemented carbide materials in a tabular form. The article also presents information on microstructural evaluation and physical and mechanical property evaluation of cemented carbides.

Coatings and thin films can be studied with surface analysis methods because their inherently small depth allows characterization of the surface composition, interface composition, and in-depth distribution of composition. This article describes principles and examples of common surface analysis methods, namely, Auger electron spectroscopy, X-ray photoelectron spectroscopy, ion scattering spectroscopy, secondary ion mass spectroscopy, and Rutherford backscattering spectroscopy. It also provides useful information on the applications of surface analysis.

This article provides a clear but nonexhaustive description of the general principle of atomic emission, with a particular focus on instrumentation, and summarizes the main characteristics of the inductively coupled plasma optical emission spectrometer technique. Basic atomic theory as well as the instrument characteristics and their influence on the instrument performances are presented. The advantages, drawbacks, and developments of this technique are discussed, and, finally, alternative techniques and examples of applications are provided.

Stainless steels are essential for the modern industrial civilization because of their corrosion resistance, especially in the chemical, petrochemical, and food industries. This article discusses the classification of the various types of stainless steels, including martensitic, ferritic, austenitic, duplex (ferritic-austenitic), and precipitation-hardening stainless steels. It presents a checklist of characteristics to be considered in selecting the proper type of stainless steel for a specific application. The article also outlines the need to promote the formation of an effective protective passive layer in stainless steels. It discusses hardness, fatigue and fretting properties, tribological properties, wear resistance, and corrosion-wear process of the S-phase layer. The article describes two thermochemical nitriding techniques of stainless steels: plasma-assisted nitriding techniques and non-plasma assisted nitriding processes. It also describes the difficulties in stainless steel nitriding/carburizing.

Low-temperature surface hardening is mostly applied to austenitic stainless steels when a combination of excellent corrosion performance and wear performance is required. This article provides a brief history of low-temperature surface hardening of stainless steel, followed by a discussion on physical metallurgy, including crystallographic identity, thermal stability and decomposition, nitrogen and carbon solubility in expanded austenite, and diffusion kinetics of interstitials. It provides a description of low-temperature nitriding and nitrocarburizing processes for primarily austenitic and, to a lesser extent, other types of stainless steels along with practical examples and industrial applications of these steels.

This article summarizes the terminology for gas reactions, and discusses low-temperature nitriding and nitrocarburizing of stainless steels. It describes the various nitriding processes, namely, high- and low-pressure nitriding, oxynitriding, sulfonitriding, oxysulfonitriding, ferritic nitrocarburizing and austenitic nitrocarburizing. The article includes a discussion on the difficulties in specimen cleaning, importance of furnace purge, uses of pre and post oxidation, depassivation, or activation, and requirements for perfect nucleation in nitriding process. In nitriding, the successful atmosphere control depends on various potentials. The article summarizes the methods of measuring potentials in nitriding and nitrocarburizing, provides useful information on the furnaces used, and the safety precautions to be followed in the nitriding process. It also describes the sample preparation procedures and testing methods to ensure the quality of the sample.

This article describes testing and characterization methods of ceramics for chemical analysis, phase analysis, microstructural analysis, macroscopic property characterization, strength and proof testing, thermophysical property testing, and nondestructive evaluation techniques. Chemical analysis is carried out by X-ray fluorescence spectrometry, atomic absorption spectrophotometry, and plasma-emission spectrophotometry. Phase analysis is done by X-ray diffraction, spectroscopic methods, thermal analysis, and quantitative analysis. Techniques used for microstructural analysis include reflected light microscopy using polarized light, scanning electron microscopy, transmission electron microscopy, energy dispersive analysis of X-rays, and wavelength dispersive analysis of X-rays. Macroscopic property characterization involves measurement of porosity, density, and surface area. The article describes testing methods such as room and high-temperature strength test methods, proof testing, fracture toughness measurement, and hardness and wear testing. It also explains methods for determining thermal expansion, thermal conductivity, heat capacity, and emissivity of ceramics and glass and measurement of these properties as a function of temperature.