1: Elemental Analysis
The purpose of elemental analysis is to determine the quantity of a particular element within a molecule or material.
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- 1.1: Introduction to Elemental Analysis
- Elemental analysis can be subdivided in two ways: Qualitative: determining what elements are present or the presence of a particular element. Quantitative: determining how much of a particular or each element is present. In either case elemental analysis is independent of structure unit or functional group.
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- 1.2: Spot Tests
- Spot tests are simple chemical procedures that uniquely identify a substance. They can be performed on small samples, even microscopic samples of matter with no preliminary separation. The first report of a spot test Hugo Shiff for the detection of uric acid. In a typical spot test, a drop of chemical reagent is added to a drop of an unknown mixture. If the substance under study is present, it produces a chemical reaction characterized by one or more unique observables, e.g., a color change.
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- 1.3: Introduction to Combustion Analysis
- Combustion analysis is a standard method of determining a chemical formula of a substance that contains hydrogen and carbon. First, a sample is weighed and then burned in a furnace in the presence of excess oxygen. All of the carbon is converted to carbon dioxide, and the hydrogen is converted to water in this way. Each of these are absorbed in separate compartments, which are weighed before and after the reaction. From these measurements, the chemical formula can be determined.
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- 1.5: ICP-AES Analysis of Nanoparticles
- ICP-AES is a spectral technique that is used to both determine the presence of metal analyte and the concentrations thereof. The ICP-AES method is introduced and a practical example is presented. This will help the reader to use this method for their own research work.
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- 1.6: ICP-MS for Trace Metal Analysis
- Inductively coupled plasma mass spectroscopy (ICP-MS) is an analytical technique for determining trace multi-elemental and isotopic concentrations in liquid, solid, or gaseous samples. It combines an ion-generating argon plasma source with the sensitive detection limit of mass spectrometry detection. Although ICP-MS is used for many different types of elemental analysis, including pharmaceutical testing and reagent manufacturing, this module will focus on mineral and water studies.
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- 1.7: Ion Selective Electrode Analysis
- Ion selective electrode (ISE) is an analytical technique used to determine the activity of ions in aqueous solution by measuring the electrical potential. ISE has many advantages compared to other techniques. Based on these advantages, ISE has wide variety of applications, which is reasonable considering the importance of measuring ion activity.
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- 1.8: A Practical Introduction to X-ray Absorption Spectroscopy
- X-ray absorption spectroscopy is a technique that uses synchrotron radiation to provide information about the electronic, structural, and magnetic properties of certain elements in materials. This information is obtained when X-rays are absorbed by an atom at energies near and above the core level binding energies of that atom. Therefore, a brief description about X-rays, synchrotron radiation and X-ray absorption is provided prior to a description of sample preparation for powdered materials.
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- 1.9: Neutron Activation Analysis (NAA)
- Neutron activation analysis (NAA) is a non-destructive analytical method commonly used to determine the identities and concentrations of elements within a variety of materials. Unlike many other analytical techniques, NAA is based on nuclear rather than electronic transitions. In NAA, samples are subjected to neutron radiation (i.e., bombarded with neutrons), which causes the elements in the sample to capture free neutrons and form radioactive isotopes.
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- 1.11: Fluorescence Spectroscopy
- Atomic fluorescence spectroscopy (AFS) is a method that was invented by Winefordner and Vickers in 1964 as a means to analyze the chemical concentration of a sample. The idea is to excite a sample vapor with the appropriate UV radiation, and by measuring the emitting radiation, the amount of the specific element being measured could be quantified.
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- 1.12: An Introduction to Energy Dispersive X-ray Spectroscopy
- Energy-dispersive X-ray spectroscopy (EDX or EDS) is an analytical technique used to probe the composition of a solid materials. Several variants exist, but the all rely on exciting electrons near the nucleus, causing more distant electrons to drop energy levels to fill the resulting “holes.”
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- 1.13: X-ray Photoelectron Spectroscopy
- X-Ray photoelectron spectroscopy (XPS), also known as electron spectroscopy for chemical analysis (ESCA), is one of the most widely used surface techniques in materials science and chemistry. It allows the determination of atomic composition of the sample in a non-destructive manner, as well as other chemical information, such as binding constants, oxidation states and speciation.
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- 1.14: Auger Electron Spectroscopy
- Auger electron spectroscopy (AES) is one of the most commonly employed surface analysis techniques. It uses the energy of emitted electrons to identify the elements present in a sample, similar to X-ray photoelectron spectroscopy (XPS). The main difference is that XPS uses an X-ray beam to eject an electron while AES uses an electron beam to eject an electron.
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- 1.15: Rutherford Backscattering of Thin Films
- One of the main research interests of the semiconductor industry is to improve the performance of semiconducting devices and to construct new materials with reduced size or thickness that have potential application in transistors and microelectronic devices. However, the most significant challenge regarding thin film semiconductor materials is measurement.
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- 1.16: An Accuracy Assessment of the Refinement of Crystallographic Positional Metal Disorder in Molecular Solid Solutions
- Crystallographic positional disorder is evident when a position in the lattice is occupied by two or more atoms; the average of which constitutes the bulk composition of the crystal. If a particular atom occupies a certain position in one unit cell and another atom occupies the same position in other unit cells, the resulting electron density will be a weight average of the situation in all the unit cells throughout the crystal.
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- 1.17: Principles of Gamma-ray Spectroscopy and Applications in Nuclear Forensics
- Gamma-ray (γ-ray) spectroscopy is a quick and nondestructive analytical technique that can be used to identify various radioactive isotopes in a sample. In gamma-ray spectroscopy, the energy of incident gamma-rays is measured by a detector.