This article presents tools, techniques, and procedures that engineers and material scientists can use to investigate plastic part failures. It also provides a brief survey of polymer systems and the key properties that need to be measured during failure analysis. It describes the characterization of plastics by infrared and nuclear magnetic resonance spectroscopy, differential scanning calorimetry, differential thermal analysis, thermogravimetric analysis, thermomechanical analysis, and dynamic mechanical analysis. The article also discusses the use of X-ray diffraction for analyzing crystal phases and structures in solid materials.

This article reviews analytical techniques that are most often used in plastic component failure analysis. The description of the techniques is intended to familiarize the reader with the general principles and benefits of the methodologies, namely Fourier transform infrared spectroscopy, energy-dispersive x-ray spectroscopy, differential scanning calorimetry, thermogravimetric analysis, and dynamic mechanical analysis. The article describes the methods for molecular weight assessment and mechanical testing to evaluate plastics and polymers. The descriptions of the analytical techniques are supplemented by a series of case studies to illustrate the significance of each method. The case studies also include pertinent visual examination results and the corresponding images that aided in the characterization of the failures.

This article discusses the operating principles, advantages, and limitations of scanning electron microscopy, atomic force microscopy, x-ray photoelectron spectroscopy, and secondary ion mass spectroscopy that are used to analyze the surface chemistry of plastics.

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.

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.

This article covers in-line process monitoring of the metal additive manufacturing (AM) methods of laser and electron beam (e-beam) powder-bed fusion (PBF) and directed-energy deposition (DED). It focuses on methods that monitor the component directly throughout the build process. This article is organized by the type of AM process and by the physics of the monitoring method. The discussion covers two types of monitoring possible with the PBF process: monitoring the area of the powder bed and component and monitoring the melt pool created by the laser or e-beam. Methods for layer monitoring include optical and thermal methods that monitor light reflected or emitted in the visible and infrared wavelengths, respectively. Monitoring methods for laser directed-energy deposition (DED) discussed are those that measure the size and shape of the melt pool, the temperature of the melt pool, and the plasma generated by the laser as it interacts with the molten metal.

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 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.

Infrared (IR) spectra have been produced by transmission, that is, transmitting light through the sample, measuring the light intensity at the detector, and comparing it to the intensity obtained with no sample in the beam, all as a function of the infrared wavelength. This article discusses the sampling techniques and applications of IR spectra as well as the molecular structure information it can provide. The discussion begins with a description of the general principle of IR spectroscopy. This is followed by a section on commercial IR instruments. Sampling techniques and accessories necessary in obtaining the infrared spectrum of a material are then discussed. The article presents various techniques and methods involved in IR qualitative analysis and quantitative analysis. It ends with a few examples of the applications of IR spectroscopy.

This article introduces the principles of Raman spectroscopy and the representative materials characterization applications to which Raman spectroscopy has been applied. A discussion on light-scattering fundamentals and a description of the experimental aspects of the technique are included. Emphasis is placed on the different instrument approaches that have been developed for performing Raman analyses on various materials. The applications presented reflect the breadth of materials characterization uses for Raman spectroscopy and highlight the analysis of bulk material and of surface and near-surface species.

This article focuses on the application of solid-state nuclear magnetic resonance (NMR) spectroscopy in materials science, especially for inorganic and organic polymer solids. It begins with a discussion on the general principles of NMR, providing information on nuclear spin descriptions and line narrowing and spectral resolution and describing the impact of magnetic field on nuclear spins and the factors determining resonance frequency. This is followed by a description of various systems and equipment necessary for NMR spectroscopy. A discussion on general sampling for solid-state NMR, sample-spinning requirements, and extraneous signals is then included. Various factors pertinent to accurate calibration of the NMR spectrum are also described. The article provides information on some of the parameters both beneficial and problematic for processing NMR data. It ends with a description of the applications of NMR in glass science and ceramics.

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.

Gas analysis by mass spectrometry, or gas mass spectrometry, is a general technique using a family of instrumentation that creates a charged ion from a gas phase chemical species and measures the mass-to-charge ratio. This article covers gas analysis applications that do not use chromatographic separation to physically isolate components of the sample prior to analysis. It is intended to provide an understanding of gas analysis instrumentation and terminology that will help make informed decisions in choosing an instrument and methodology appropriate for the data needed. Mass-analyzer technologies for gas mass spectrometry, namely quadrupole mass filters, magnetic sector mass filters, and time-of-flight mass analyzers are covered. Common factors to consider in choosing an analyzer for static or continuous gas measurement are also described. In addition, the article presents some examples of applications of gas mass spectrometry.

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 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 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 is a brief account of low-energy ion-scattering spectroscopy (LEIS) for determining the atomic structure of solid surfaces. It begins with a description of the general principles of LEIS. This is followed by a section providing information on the equipment used for LEIS. Various steps involved in the sample preparation, calibration, and data analysis are then discussed. The article concludes with a section on the applications and interpretation of LEIS in material analysis, including discussion on surface structural analysis, layer-by-layer (Frank-van der Merwe) growth, and low-energy atom-scattering spectroscopy.

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 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.