Sample preparation

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In analytical chemistry, sample preparation (working-up) refers to the ways in which a sample is treated prior to its analyses. Preparation is a very important step in most analytical techniques, because the techniques are often not responsive to the analyte in its in-situ form, or the results are distorted by interfering species. Sample preparation may involve dissolution, extraction, reaction with some chemical species, pulverizing, treatment with a chelating agent (e.g. EDTA), masking, filtering, dilution, sub-sampling or many other techniques. Treatment is done to prepare the sample into a form ready for analysis by specified analytical equipment. Sample preparation could involve: crushing and dissolution, chemical digestion with acid or alkali, sample extraction, sample clean up and sample pre-concentration.

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<span class="mw-page-title-main">Analytical chemistry</span> Study of the separation, identification, and quantification of the chemical components of materials

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<span class="mw-page-title-main">Neutron activation analysis</span>

Neutron activation analysis (NAA) is the nuclear process used for determining the concentrations of elements in many materials. NAA allows discrete sampling of elements as it disregards the chemical form of a sample, and focuses solely on atomic nuclei. The method is based on neutron activation and thus requires a source of neutrons. The sample is bombarded with neutrons, causing its constituent elements to form radioactive isotopes. The radioactive emissions and radioactive decay paths for each element have long been studied and determined. Using this information, it is possible to study spectra of the emissions of the radioactive sample, and determine the concentrations of the various elements within it. A particular advantage of this technique is that it does not destroy the sample, and thus has been used for the analysis of works of art and historical artifacts. NAA can also be used to determine the activity of a radioactive sample.

<span class="mw-page-title-main">Gravimetric analysis</span> Quantitative determination of a chemical species based on its mass

Gravimetric analysis describes a set of methods used in analytical chemistry for the quantitative determination of an analyte based on its mass. The principle of this type of analysis is that once an ion's mass has been determined as a unique compound, that known measurement can then be used to determine the same analyte's mass in a mixture, as long as the relative quantities of the other constituents are known.

Coulometry determines the amount of matter transformed during an electrolysis reaction by measuring the amount of electricity consumed or produced. It can be used for precision measurements of charge, and the amperes even used to have a coulometric definition. However, today coulometry is mainly used for analytical applications. Coulometry is a group of techniques in analytical chemistry. It is named after Charles-Augustin de Coulomb.

Supercritical fluid extraction (SFE) is the process of separating one component (the extractant) from another (the matrix) using supercritical fluids as the extracting solvent. Extraction is usually from a solid matrix, but can also be from liquids. SFE can be used as a sample preparation step for analytical purposes, or on a larger scale to either strip unwanted material from a product (e.g. decaffeination) or collect a desired product (e.g. essential oils). These essential oils can include limonene and other straight solvents. Carbon dioxide (CO2) is the most used supercritical fluid, sometimes modified by co-solvents such as ethanol or methanol. Extraction conditions for supercritical carbon dioxide are above the critical temperature of 31 °C and critical pressure of 74 bar. Addition of modifiers may slightly alter this. The discussion below will mainly refer to extraction with CO2, except where specified.

<span class="mw-page-title-main">AutoAnalyzer</span> Automated analyzer using a flow technique

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<span class="mw-page-title-main">Solid-phase extraction</span> Process to separate compounds by properties

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Environmental monitoring describes the processes and activities that need to take place to characterize and monitor the quality of the environment. Environmental monitoring is used in the preparation of environmental impact assessments, as well as in many circumstances in which human activities carry a risk of harmful effects on the natural environment. All monitoring strategies and programs have reasons and justifications which are often designed to establish the current status of an environment or to establish trends in environmental parameters. In all cases, the results of monitoring will be reviewed, analyzed statistically, and published. The design of a monitoring program must therefore have regard to the final use of the data before monitoring starts.

Bioanalysis is a sub-discipline of analytical chemistry covering the quantitative measurement of xenobiotics and biotics in biological systems.

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Water chemistry analyses are carried out to identify and quantify the chemical components and properties of water samples. The type and sensitivity of the analysis depends on the purpose of the analysis and the anticipated use of the water. Chemical water analysis is carried out on water used in industrial processes, on waste-water stream, on rivers and stream, on rainfall and on the sea. In all cases the results of the analysis provides information that can be used to make decisions or to provide re-assurance that conditions are as expected. The analytical parameters selected are chosen to be appropriate for the decision making process or to establish acceptable normality. Water chemistry analysis is often the groundwork of studies of water quality, pollution, hydrology and geothermal waters. Analytical methods routinely used can detect and measure all the natural elements and their inorganic compounds and a very wide range of organic chemical species using methods such as gas chromatography and mass spectrometry. In water treatment plants producing drinking water and in some industrial processes using products with distinctive taste and odours, specialised organoleptic methods may be used to detect smells at very low concentrations.

<span class="mw-page-title-main">Extraction (chemistry)</span> Separation of a desired substance from other substances in the sample

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<span class="mw-page-title-main">Extractive electrospray ionization</span>

Extractive electrospray ionization (EESI) is a spray-type, ambient ionization source in mass spectrometry that uses two colliding aerosols, one of which is generated by electrospray. In standard EESI, syringe pumps provide the liquids for both an electrospray and a sample spray. In neutral desorption EESI (ND-EESI), the liquid for the sample aerosol is provided by a flow of nitrogen.

Ion suppression in LC-MS and LC-MS/MS refers to reduced detector response, or signal:noise as a manifested effect of competition for ionisation efficiency in the ionisation source, between the analyte(s) of interest and other endogenous or exogenous species which have not been removed from the sample matrix during sample preparation. Ion suppression is not strictly a problem unless interfering compounds elute at the same time as the analyte of interest. In cases where ion suppressing species do co-elute with an analyte, the effects on the important analytical parameters including precision, accuracy and limit of detection can be extensive, severely limiting the validity of an assay's results.

Electro membrane extraction, or EME, is a miniaturized liquid-liquid extraction technique developed for sample preparation of aqueous samples prior to analysis by chromatography, electrophoresis, mass spectrometry, and related techniques in analytical chemistry. EME involves the use of a small supported liquid membrane (SLM) sustained in the wall of a porous hollow fiber, and application of an electrical field across the SLM.

Accelerated solvent extraction (ASE) is a method for extracting various chemicals from a complex solid or semisolid sample matrix. The process uses high temperature and pressure, which results in the extraction taking less time and requiring less solvent, and possibly also giving better analyte recovery, than traditional methods that use less extreme conditions. The elevated temperature is employed to increase extraction efficiency of the analyte of interest and the elevated pressure is used to keep the solvent in a liquid state as the temperature is increased above its boiling point. An automated system for the process was developed by Dionex, a company owned by Thermo Fisher Scientific.

Single-drop microextraction (SDME) is a sample preparation technique in chemical test or analytical chemistry. SDME uses only a single drop of solvent to isolate and preconcentrate analytes from a sample matrix. The extremely low solvent use of SDME makes it cost-effective and less harmful to the environment, subscribing to the principles of green analytical chemistry.

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