Microanalysis
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Microanalysis
Microanalysis is the chemical identification and quantitative analysis of very small amounts of chemical substances (generally less than 10 mg or 1 ml) or very small surfaces of material (generally less than 1 cm2). One of the pioneers in the microanalysis of chemical elements was the Austrian Nobel Prize winner Fritz Pregl.http://nobelprize.org/nobel_prizes/chemistry/laureates/1923/index.html ''The Nobel Prize in Chemistry 1923''. Nobelprize.org. Retrieved 2014-08-06 Methods The most known methods used in microanalysis include: * Most of the spectroscopy methods: ultraviolet–visible spectroscopy, infrared spectroscopy, nuclear magnetic resonance, X-ray fluorescence, Energy-dispersive X-ray spectroscopy, Wavelength-dispersive X-ray spectroscopy, and mass spectrometry * Most of the chromatography methods : high-performance liquid chromatography, Gel permeation chromatography; * Some thermal analysis methods: differential scanning calorimetry, thermogravimetric analy ...
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X-ray Fluorescence
X-ray fluorescence (XRF) is the emission of characteristic "secondary" (or fluorescent) X-rays from a material that has been excited by being bombarded with high-energy X-rays or gamma rays. The phenomenon is widely used for elemental analysis and analytical chemistry, chemical analysis, particularly in the investigation of metals, glass, ceramics and building materials, and for research in geochemistry, forensic science, archaeology and art objects such as paintings. Underlying physics When materials are exposed to short-wavelength X-rays or to gamma rays, ionization of their component atoms may take place. Ionization consists of the ejection of one or more electrons from the atom, and may occur if the atom is exposed to radiation with an energy greater than its ionization energy. X-rays and gamma rays can be energetic enough to expel tightly held electrons from the inner atomic orbital, orbitals of the atom. The removal of an electron in this way makes the electronic structu ...
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Wavelength-dispersive X-ray Spectroscopy
Wavelength-dispersive X-ray spectroscopy (WDXS or WDS) is a non-destructive analysis technique used to obtain elemental information about a range of materials by measuring characteristic x-rays within a small wavelength range. The technique generates a spectrum in which the peaks correspond to specific x-ray lines and elements can be easily identified. WDS is primarily used in chemical analysis, wavelength dispersive X-ray fluorescence (WDXRF) spectrometry, electron microprobes, scanning electron microscopes, and high precision experiments for testing atomic and plasma physics. Theory Wavelength-dispersive X-ray spectroscopy is based on known principles of how the characteristic x-rays are generated by a sample and how the x-rays are measured. X-ray generation X-rays are generated when an electron beam of high enough energy dislodges an electron from an inner orbital within an atom or ion, creating a void. This void is filled when an electron from a higher orbital release ...
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Energy-dispersive X-ray Spectroscopy
Energy-dispersive X-ray spectroscopy (EDS, EDX, EDXS or XEDS), sometimes called energy dispersive X-ray analysis (EDXA or EDAX) or energy dispersive X-ray microanalysis (EDXMA), is an analytical technique used for the elemental analysis or chemical characterization of a sample. It relies on an interaction of some source of X-ray excitation and a sample. Its characterization capabilities are due in large part to the fundamental principle that each element has a unique atomic structure allowing a unique set of peaks on its electromagnetic emission spectrum (which is the main principle of spectroscopy). The peak positions are predicted by the Moseley's law with accuracy much better than experimental resolution of a typical EDX instrument. To stimulate the emission of characteristic X-rays from a specimen a beam of electrons is focused into the sample being studied. At rest, an atom within the sample contains ground state (or unexcited) electrons in discrete energy levels or electron ...
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Quantitative Analysis (chemistry)
In analytical chemistry, quantitative analysis is the determination of the absolute or relative abundance (often expressed as a concentration) of one, several or all particular substance(s) present in a sample. Methods Once the presence of certain substances in a sample is known, the study of their absolute or relative abundance could help in determining specific properties. Knowing the composition of a sample is very important, and several ways have been developed to make it possible, like gravimetric and volumetric analysis. Gravimetric analysis yields more accurate data about the composition of a sample than volumetric analysis but also takes more time to perform in the laboratory. Volumetric analysis, on the other hand, doesn't take that much time and can produce satisfactory results. Volumetric analysis can be simply a titration based in a neutralization reaction but it can also be a precipitation or a complex forming reaction as well as a titration based in a redox reactio ...
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High-performance Liquid Chromatography
High-performance liquid chromatography (HPLC), formerly referred to as high-pressure liquid chromatography, is a technique in analytical chemistry used to separate, identify, and quantify each component in a mixture. It relies on pumps to pass a pressurized liquid solvent containing the sample mixture through a column filled with a solid adsorbent material. Each component in the sample interacts slightly differently with the adsorbent material, causing different flow rates for the different components and leading to the separation of the components as they flow out of the column. HPLC has been used for manufacturing (''e.g.'', during the production process of pharmaceutical and biological products), legal (''e.g.'', detecting performance enhancement drugs in urine), research (''e.g.'', separating the components of a complex biological sample, or of similar synthetic chemicals from each other), and medical (''e.g.'', detecting vitamin D levels in blood serum) purposes. Chrom ...
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Combustion Analysis
Combustion analysis is a method used in both organic chemistry and analytical chemistry to determine the elemental composition (more precisely empirical formula) of a pure organic compound by combusting the sample under conditions where the resulting combustion products can be quantitatively analyzed. Once the number of moles of each combustion product has been determined the empirical formula or a partial empirical formula of the original compound can be calculated. Applications for combustion analysis involve only the elements of carbon (C), hydrogen (H), nitrogen (N), and sulfur (S) as combustion of materials containing them convert these elements to their oxidized form (CO2, H2O, NO or NO2, and SO2) under high temperature high oxygen conditions. Notable interests for these elements involve measuring total nitrogen in food or feed to determine protein percentage, measuring sulfur in petroleum products, or measuring total organic carbon (TOC) in water. History The method was ...
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X-ray Diffraction
X-ray crystallography is the experimental science determining the atomic and molecular structure of a crystal, in which the crystalline structure causes a beam of incident X-rays to diffract into many specific directions. By measuring the angles and intensities of these diffracted beams, a crystallographer can produce a three-dimensional picture of the density of electrons within the crystal. From this electron density, the mean positions of the atoms in the crystal can be determined, as well as their chemical bonds, their crystallographic disorder, and various other information. Since many materials can form crystals—such as salts, metals, minerals, semiconductors, as well as various inorganic, organic, and biological molecules—X-ray crystallography has been fundamental in the development of many scientific fields. In its first decades of use, this method determined the size of atoms, the lengths and types of chemical bonds, and the atomic-scale differences among various mat ...
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Field Flow Fractionation
Field-flow fractionation, abbreviated FFF, is a separation technique which does not have a stationary phase. It is similar to liquid chromatography as it works on dilute solutions or suspensions of the solute. Separation is achieved by applying a field (hydraulic, centrifugal, thermal, electric, magnetic, gravitational, ...) perpendicular to the direction of transport of the sample which is pumped through a long and narrow channel. The field exerts a force on the sample components concentrating them towards one of the channel walls, which is called accumulation wall. The force interacts with a property of the sample on which then the separation occurs, in other words on their differing "mobilities" under the force exerted by the field. As an example, for the hydraulic, or cross-flow FFF method, the property driving separation is the translational diffusion coefficient or the hydrodynamic size. For a thermal field (heating one wall and cooling the other), it is the ratio of the t ...
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Electrophoresis
Electrophoresis, from Ancient Greek ἤλεκτρον (ḗlektron, "amber") and φόρησις (phórēsis, "the act of bearing"), is the motion of dispersed particles relative to a fluid under the influence of a spatially uniform electric field. Electrophoresis of positively charged particles (cations) is sometimes called cataphoresis, while electrophoresis of negatively charged particles (anions) is sometimes called anaphoresis. The electrokinetic phenomenon of electrophoresis was observed for the first time in 1807 by Russian professors Peter Ivanovich Strakhov and Ferdinand Frederic Reuss at Moscow University, who noticed that the application of a constant electric field caused clay particles dispersed in water to migrate. It is ultimately caused by the presence of a charged interface between the particle surface and the surrounding fluid. It is the basis for analytical techniques used in chemistry for separating molecules by size, charge, or binding affinity. Electropho ...
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Thermogravimetric Analysis
Thermogravimetric analysis or thermal gravimetric analysis (TGA) is a method of thermal analysis in which the mass of a sample is measured over time as the temperature changes. This measurement provides information about physical phenomena, such as phase transitions, absorption, adsorption and desorption; as well as chemical phenomena including chemisorptions, thermal decomposition, and solid-gas reactions (e.g., oxidation or reduction). Thermogravimetric analyzer Thermogravimetric analysis (TGA) is conducted on an instrument referred to as a thermogravimetric analyzer. A thermogravimetric analyzer continuously measures mass while the temperature of a sample is changed over time. Mass, temperature, and time are considered base measurements in thermogravimetric analysis while many additional measures may be derived from these three base measurements. A typical thermogravimetric analyzer consists of a precision balance with a sample pan located inside a furnace with a programmab ...
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Differential Scanning Calorimetry
Differential scanning calorimetry (DSC) is a thermoanalytical technique in which the difference in the amount of heat required to increase the temperature of a sample and reference is measured as a function of temperature. Both the sample and reference are maintained at nearly the same temperature throughout the experiment. Generally, the temperature program for a DSC analysis is designed such that the sample holder temperature increases linearly as a function of time. The reference sample should have a well-defined heat capacity over the range of temperatures to be scanned. The technique was developed by E. S. Watson and M. J. O'Neill in 1962, and introduced commercially at the 1963 Pittsburgh Conference on Analytical Chemistry and Applied Spectroscopy. The first adiabatic differential scanning calorimeter that could be used in biochemistry was developed by P. L. Privalov and D. R. Monaselidze in 1964 at Institute of Physics in Tbilisi, Georgia. The term DSC was coined to descr ...
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Thermal Analysis
Thermal analysis is a branch of materials science where the properties of materials are studied as they change with temperature. Several methods are commonly used – these are distinguished from one another by the property which is measured: * Dielectric thermal analysis: dielectric permittivity and loss factor * Differential thermal analysis: temperature difference versus temperature or time * Differential scanning calorimetry: heat flow changes versus temperature or time * Dilatometer, Dilatometry: volume changes with temperature change * Dynamic mechanical analysis: measures storage modulus (stiffness) and loss modulus (damping) versus temperature, time and frequency * Evolved gas analysis: analysis of gases evolved during heating of a material, usually decomposition products * Isothermal titration calorimetry * Isothermal microcalorimetry * Laser flash analysis: thermal diffusivity and thermal conductivity * Thermogravimetric analysis: mass change versus temperature or time ...
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