Search Results for qualitative 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 provides a detailed account of the principles, instrumentation,and applications of x-ray photoelectron spectroscopy (XPS), a technique used for elemental and compositional analysis of surfaces and thin films. It reviews the nomenclature of energy states and sensitivity of electrons at the surface that are capable of producing peaks in XPS. Additionally, it presents information on the instrumentation and the preparation and mounting of samples for XPS analysis. The article explains qualitative analysis, namely, measuring of shifts in the binding energy of core electrons, multiplet splitting, and the Auger parameter; and quantitative analysis such as depth analysis carried out using XPS. It also discusses the applications of XPS with examples.

Infrared (IR) spectroscopy is a useful technique for characterizing materials and providing information on the molecular structure, dynamics, and environment of a compound. This article provides the basic principles and instrumentation of IR spectroscopy. It discusses the sampling techniques of IR spectroscopy, namely, attenuated total reflectance spectroscopy, diffuse reflectance spectroscopy, infrared reflection-absorption spectroscopy, emission spectroscopy, and photoacoustic spectroscopy, and chromatographic techniques. Explaining the qualitative analysis of IR spectroscopy, the article provides information on spectral absorbance-subtraction, analysis of components in spectral matrix mixture, and determination of exact peak location of broad profiles. It discusses the quantitative analysis that mainly includes Beer's law for single compound in single wave number. The article also exemplifies the applications of IR spectroscopy.

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.

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 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 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.

Thermoelastic stress analysis (TSA) an increasingly popular infrared (IR)-based technique for measuring stress on the surface of a part subjected to time-varying loads. This article begins by providing a theoretical and historical background of thermoelastic stress analysis. It then describes infrared detectors, such as quantum detectors and thermal/nonquantum detectors, for thermoelastic stress analysis. The article discusses the theoretical aspects for producing thermoelastic stress analysis data and the applications amenable to thermoelastic stress analysis. It concludes with information on the qualitative applications of thermoelastic stress analysis.

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 presumes the reader has a basic understanding of the operation and principles of scanning electron microscopy (SEM). The emphasis of this article is specifically on the application of SEM to the study of metallic and nonmetallic fracture surfaces, where the typical objectives of SEM examination of a fracture surface may include the following: identification of characteristic fracture features to aid in identifying fracture mechanism(s); characterization of material anomalies that may have influenced the fracture; qualitative or semiquantitative chemical analysis of component material(s); and qualitative or semiquantitative analysis of deposits or corrosion products on or near fracture surfaces.

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.

Risk and hazard analysis can be effectively used during design reviews to provide valuable feedback to the design to avoid failures. This article discusses the types of risks, namely, real risk, statistical risk, predicted risk, and perceived risk. It describes the principle and technical methods of risk/hazard analysis practiced in the industry to identify possible hazards and the resources necessary to avoid or reduce risks. These methods include the failure mode and effect analysis, fault tree analysis, event tree analysis, risk/benefit analysis, safety analysis, and probabilistic estimates.

Several qualitative, semiquantitative, and quantitative tests are available to estimate and control metal cleanliness, particularly inclusion concentration of aluminum alloys. This article provides a description of a few of the metal cleanliness assessment techniques, such as chemical analysis, pressure filter tests, electric resistivity tests, reduced-pressure test, and ultrasonic technique. Detection methods based on the certain principles and the types of impurities in chemical analysis are discussed.

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.

Microstructural analysis is the combined characterization of the morphology, elemental composition, and crystallography of microstructural features through the use of a microscope. This article reviews three types of the most commonly used electron microscopies in metallurgical studies, namely scanning electron microscopy, electron probe microanalysis, and transmission electron microscopy. It briefly describes the operating principles, instrumentation which includes energy dispersive X-ray detectors, spatial resolution, typical use of the techniques, elemental analysis detection threshold and precision, limitations, sample requirements, and the capabilities of related techniques.

This article provides an overview of the general methods of metal powder production. It details the primary methods for particle sizing used in additive manufacturing: sieving, laser diffraction and scattering, and digital image analysis. Methods of interpreting and understanding particle size distribution (PSD) data are presented, with an emphasis on the differences between count- and volume-based PSDs. The article then outlines practices for both qualitative and quantitative assessment of particle morphology.

This article introduces various analytical techniques commonly used in the characterization of organic solids and liquids and discusses the challenges in performing the analysis, with examples. Some general advice in approaching a material analysis is also provided.

This article provides an introduction to the molecular fluorescence spectroscopy, and discusses the theory of fluorescence and its application to chemical analysis. It provides information on fluorescence that occurs in organic compounds and inorganic atoms and molecules. The article describes the instruments used in the spectroscopy, namely, radiation sources, sample holders, wavelength selectors, detectors, computers, and ratiometric instruments. The practical considerations include solvent effects, corrected spectra, wavelength calibration, temperature, and scattered light. The article also discusses the uses of some special techniques used in molecular fluorescence spectroscopy.