This article provides a detailed account of X-ray spectroscopy used for elemental identification and determination. It begins with an overview of the operating principles of X-ray fluorescence (XRF) spectrometer, as well as a comparison of the operating principles of wavelength-dispersive spectrometer (WDS) and energy-dispersive spectrometer (EDS). This is followed by a discussion on the mechanism and effects of X-ray radiation, X-ray emission, and X-ray absorption. The article then discusses components used, operation, and applications of WDS and EDS. Some of the factors and processes involved in sample preparation for XRF analysis are also included. The article further provides information on the practical procedure for and the applications of WDS and EDS qualitative and quantitative analyses.

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.

Electron probe microanalysis (EPMA) makes it possible to combine structural and compositional analysis in one operation. This article describes the basic concepts of microanalysis and the processing of EPMA that involves the measurement of the characteristic X-rays emitted from a microscopic part of a solid specimen bombarded by a beam of accelerated electrons. It provides information on the various aspects of energy-dispersive spectrometry (EDS) and wavelength-dispersive spectrometry (WDS), and elucidates the qualitative analysis of the major constituents of EDS and WDS. The article includes information on the analog and digital compositional mapping of elemental distribution, and describes the strengths and weaknesses of WDS and EDS spectrometers in X-ray mapping. It also outlines the application of EPMA for solving various problems in materials science.

The overall chemical composition of metals and alloys is most commonly determined by X-ray fluorescence (XRF) and optical emission spectroscopy (OES), and combustion and inert gas fusion analysis. This article provides information on the capabilities, uses, detection threshold and precision methods, and sample requirements. The amount of material that needs to be sampled, operating principles, and limitations of the stated methods are also discussed.

This article provides an introduction to x-ray spectrometry, and discusses the role of electromagnetic radiation, x-ray emission, and x-ray absorption. It focuses on the instrumentation of wavelength-dispersive x-ray spectrometers, and energy dispersive x-ray spectrometers (EDS) that comprise x-ray tubes, the analyzing system, and detectors. The fundamentals of EDS operation are described. The article also provides useful information on preparation of various samples, explaining the qualitative and quantitative analyses of EDS. It reviews the applications of the x-ray spectrometry.

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.

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.

Inductively coupled plasma atomic emission spectroscopy (ICP-AES) is an analytical technique for elemental determinations in the concentration range of major to trace based on the principles of atomic spectroscopy. This article provides a description of the basic atomic theory, and explains the analytical procedures and various interference effects of ICP, namely, spectral, vaporization-atomization, and ionization. It provides a detailed discussion on the principal components of an analytical ICP system, namely, the sample introduction system; ICP torch and argon gas supplies; radio-frequency generator and associated electronics; spectrometers, such as polychromators and monochromators; detection electronics and interface; and the system computer with appropriate hardware and software. The article also describes the uses of direct-current plasma, and provides examples of the applications of ICP-AES.

This article outlines the beam/sample interactions and the basic instrumental design of a scanning electron microscopy (SEM), which include the electron gun, probeforming column (consisting of magnetic electron lenses, apertures, and scanning coils), electron detectors, and vacuum system. It discusses the contrasts mechanisms used for imaging and analyzing materials in the SEM. These include the topographic contrast, compositional contrast, and electron channeling pattern and orientation contrast. Special instrumentation and accessory equipment used at elevated pressures and during the X-ray microanalysis are reviewed. The article also provides information on the sample preparation procedure and the materials applications of the SEM.