Analytical technique

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Analytical technique is a method used to determine a chemical or physical property of a chemical substance, chemical element, or mixture. [1] There is a wide variety of techniques used for analysis, from simple weighing to advanced techniques using highly specialized instrumentation.

Contents

Classical methods of analysis

Classical analysis methods involve basic analytical methods widely used in laboratories. Gravimetric analysis measures the weight of the sample. Titrimetry is a family of techniques used to determine the concentration of an analyte. [2]

Spectrochemical analysis

Spectrometer can determine chemical composition through its measure of spectrums. The common spectrometer used in analytical chemistry is Mass spectrometry. In a mass spectrometer, a small amount of sample is ionized and converted to gaseous ions, where they are separated and analyzed according to their mass-to-charge ratios. [2]

NMR Spectroscopy involves exciting a NMR-active sample and then measuring the effects of this magnetic excitation. From this, the bonds present in a sample can be determined.

Electroanalytical analysis

Electroanalytical methods utilize the potential or current of a electrochemical cell. The three main sections of this type of analysis are potentiometry, coulometry and voltammetry. Potentiometry measures the cell's potential, coulometry measures the cell's current, and voltammetry measures the change in current when cell potential changes. [3] [4]

Chromatography

Chromatography separates the analyte from the rest of the sample so that it may be measured without interference from other compounds. [2] There are different types of chromatography that differ from the media they use to separate the analyte and the sample. [5] In Thin-layer chromatography, the analyte mixture moves up and separates along the coated sheet under the volatile mobile phase. In Gas chromatography, gas separates the volatile analytes. A common method for chromatography using liquid as a mobile phase is High-performance liquid chromatography.

See also

Related Research Articles

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

Analytical chemistry studies and uses instruments and methods to separate, identify, and quantify matter. In practice, separation, identification or quantification may constitute the entire analysis or be combined with another method. Separation isolates analytes. Qualitative analysis identifies analytes, while quantitative analysis determines the numerical amount or concentration.

<span class="mw-page-title-main">Electron ionization</span> Ionization technique

Electron ionization is an ionization method in which energetic electrons interact with solid or gas phase atoms or molecules to produce ions. EI was one of the first ionization techniques developed for mass spectrometry. However, this method is still a popular ionization technique. This technique is considered a hard ionization method, since it uses highly energetic electrons to produce ions. This leads to extensive fragmentation, which can be helpful for structure determination of unknown compounds. EI is the most useful for organic compounds which have a molecular weight below 600. Also, several other thermally stable and volatile compounds in solid, liquid and gas states can be detected with the use of this technique when coupled with various separation methods.

<span class="mw-page-title-main">Gas chromatography</span> Type of chromatography

Gas chromatography (GC) is a common type of chromatography used in analytical chemistry for separating and analyzing compounds that can be vaporized without decomposition. Typical uses of GC include testing the purity of a particular substance, or separating the different components of a mixture. In preparative chromatography, GC can be used to prepare pure compounds from a mixture.

<span class="mw-page-title-main">Gas chromatography–mass spectrometry</span> Analytical method

Gas chromatography–mass spectrometry (GC–MS) is an analytical method that combines the features of gas-chromatography and mass spectrometry to identify different substances within a test sample. Applications of GC–MS include drug detection, fire investigation, environmental analysis, explosives investigation, food and flavor analysis, and identification of unknown samples, including that of material samples obtained from planet Mars during probe missions as early as the 1970s. GC–MS can also be used in airport security to detect substances in luggage or on human beings. Additionally, it can identify trace elements in materials that were previously thought to have disintegrated beyond identification. Like liquid chromatography–mass spectrometry, it allows analysis and detection even of tiny amounts of a substance.

<span class="mw-page-title-main">Metabolomics</span> Scientific study of chemical processes involving metabolites

Metabolomics is the scientific study of chemical processes involving metabolites, the small molecule substrates, intermediates, and products of cell metabolism. Specifically, metabolomics is the "systematic study of the unique chemical fingerprints that specific cellular processes leave behind", the study of their small-molecule metabolite profiles. The metabolome represents the complete set of metabolites in a biological cell, tissue, organ, or organism, which are the end products of cellular processes. Messenger RNA (mRNA), gene expression data, and proteomic analyses reveal the set of gene products being produced in the cell, data that represents one aspect of cellular function. Conversely, metabolic profiling can give an instantaneous snapshot of the physiology of that cell, and thus, metabolomics provides a direct "functional readout of the physiological state" of an organism. There are indeed quantifiable correlations between the metabolome and the other cellular ensembles, which can be used to predict metabolite abundances in biological samples from, for example mRNA abundances. One of the ultimate challenges of systems biology is to integrate metabolomics with all other -omics information to provide a better understanding of cellular biology.

<span class="mw-page-title-main">Cyclic voltammetry</span> Method of analyzing electrochemical reactions

In electrochemistry, cyclic voltammetry (CV) is a type of potentiodynamic measurement. In a cyclic voltammetry experiment, the working electrode potential is ramped linearly versus time. Unlike in linear sweep voltammetry, after the set potential is reached in a CV experiment, the working electrode's potential is ramped in the opposite direction to return to the initial potential. These cycles of ramps in potential may be repeated as many times as needed. The current at the working electrode is plotted versus the applied voltage to give the cyclic voltammogram trace. Cyclic voltammetry is generally used to study the electrochemical properties of an analyte in solution or of a molecule that is adsorbed onto the electrode.

<span class="mw-page-title-main">Elemental analysis</span> Process of analytical chemistry

Elemental analysis is a process where a sample of some material is analyzed for its elemental and sometimes isotopic composition. Elemental analysis can be qualitative, and it can be quantitative. Elemental analysis falls within the ambit of analytical chemistry, the instruments involved in deciphering the chemical nature of our world.

<span class="mw-page-title-main">Liquid chromatography–mass spectrometry</span> Analytical chemistry technique

Liquid chromatography–mass spectrometry (LC–MS) is an analytical chemistry technique that combines the physical separation capabilities of liquid chromatography with the mass analysis capabilities of mass spectrometry (MS). Coupled chromatography - MS systems are popular in chemical analysis because the individual capabilities of each technique are enhanced synergistically. While liquid chromatography separates mixtures with multiple components, mass spectrometry provides spectral information that may help to identify each separated component. MS is not only sensitive, but provides selective detection, relieving the need for complete chromatographic separation. LC–MS is also appropriate for metabolomics because of its good coverage of a wide range of chemicals. This tandem technique can be used to analyze biochemical, organic, and inorganic compounds commonly found in complex samples of environmental and biological origin. Therefore, LC–MS may be applied in a wide range of sectors including biotechnology, environment monitoring, food processing, and pharmaceutical, agrochemical, and cosmetic industries. Since the early 2000s, LC–MS has also begun to be used in clinical applications.

<span class="mw-page-title-main">Voltammetry</span> Method of analyzing electrochemical reactions

Voltammetry is a category of electroanalytical methods used in analytical chemistry and various industrial processes. In voltammetry, information about an analyte is obtained by measuring the current as the potential is varied. The analytical data for a voltammetric experiment comes in the form of a voltammogram, which plots the current produced by the analyte versus the potential of the working electrode.

<span class="mw-page-title-main">Chronoamperometry</span> Analytical method in electrochemistry

In electrochemistry, chronoamperometry is an analytical technique in which the electric potential of the working electrode is stepped and the resulting current from faradaic processes occurring at the electrode is monitored as a function of time. The functional relationship between current response and time is measured after applying single or double potential step to the working electrode of the electrochemical system. Limited information about the identity of the electrolyzed species can be obtained from the ratio of the peak oxidation current versus the peak reduction current. However, as with all pulsed techniques, chronoamperometry generates high charging currents, which decay exponentially with time as any RC circuit. The Faradaic current - which is due to electron transfer events and is most often the current component of interest - decays as described in the Cottrell equation. In most electrochemical cells, this decay is much slower than the charging decay-cells with no supporting electrolyte are notable exceptions. Most commonly a three-electrode system is used. Since the current is integrated over relatively longer time intervals, chronoamperometry gives a better signal-to-noise ratio in comparison to other amperometric techniques.

In a chemical analysis, the internal standard method involves adding the same amount of a chemical substance to each sample and calibration solution. The internal standard responds proportionally to changes in the analyte and provides a similar, but not identical, measurement signal. It must also be absent from the sample matrix to ensure there is no other source of the internal standard present. Taking the ratio of analyte signal to internal standard signal and plotting it against the analyte concentrations in the calibration solutions will result in a calibration curve. The calibration curve can then be used to calculate the analyte concentration in an unknown sample.

<span class="mw-page-title-main">Thermospray</span>

Thermospray is a soft ionization source by which a solvent flow of liquid sample passes through a very thin heated column to become a spray of fine liquid droplets. As a form of atmospheric pressure ionization in mass spectrometry these droplets are then ionized via a low-current discharge electrode to create a solvent ion plasma. A repeller then directs these charged particles through the skimmer and acceleration region to introduce the aerosolized sample to a mass spectrometer. It is particularly useful in liquid chromatography-mass spectrometry (LC-MS).

Electroanalytical methods are a class of techniques in analytical chemistry which study an analyte by measuring the potential (volts) and/or current (amperes) in an electrochemical cell containing the analyte. These methods can be broken down into several categories depending on which aspects of the cell are controlled and which are measured. The four main categories are potentiometry, amperometry, coulometry, and voltammetry.

Sample preparation for mass spectrometry is used for the optimization of a sample for analysis in a mass spectrometer (MS). Each ionization method has certain factors that must be considered for that method to be successful, such as volume, concentration, sample phase, and composition of the analyte solution. Quite possibly the most important consideration in sample preparation is knowing what phase the sample must be in for analysis to be successful. In some cases the analyte itself must be purified before entering the ion source. In other situations, the matrix, or everything in the solution surrounding the analyte, is the most important factor to consider and adjust. Often, sample preparation itself for mass spectrometry can be avoided by coupling mass spectrometry to a chromatography method, or some other form of separation before entering the mass spectrometer. In some cases, the analyte itself must be adjusted so that analysis is possible, such as in protein mass spectrometry, where usually the protein of interest is cleaved into peptides before analysis, either by in-gel digestion or by proteolysis in solution.

<span class="mw-page-title-main">Two-dimensional chromatography</span>

Two-dimensional chromatography is a type of chromatographic technique in which the injected sample is separated by passing through two different separation stages. Two different chromatographic columns are connected in sequence, and the effluent from the first system is transferred onto the second column. Typically the second column has a different separation mechanism, so that bands that are poorly resolved from the first column may be completely separated in the second column. Alternately, the two columns might run at different temperatures. During the second stage of separation the rate at which the separation occurs must be faster than the first stage, since there is still only a single detector. The plane surface is amenable to sequential development in two directions using two different solvents.

In analytical chemistry, hydrodynamic voltammetry is a form of voltammetry in which the analyte solution flows relative to a working electrode. In many voltammetry techniques, the solution is intentionally left still to allow diffusion-controlled mass transfer. When a solution is made to flow, through stirring or some other physical mechanism, it is very important to the technique to achieve a very controlled flux or mass transfer in order to obtain predictable results. These methods are types of electrochemical studies which use potentiostats to investigate reaction mechanisms related to redox chemistry among other chemical phenomenon.

Bulk electrolysis is also known as potentiostatic coulometry or controlled potential coulometry. The experiment is a form of coulometry which generally employs a three electrode system controlled by a potentiostat. In the experiment the working electrode is held at a constant potential (volts) and current (amps) is monitored over time (seconds). In a properly run experiment an analyte is quantitatively converted from its original oxidation state to a new oxidation state, either reduced or oxidized. As the substrate is consumed, the current also decreases, approaching zero when the conversion nears completion.

<span class="mw-page-title-main">Triple quadrupole mass spectrometer</span>

A triple quadrupole mass spectrometer (TQMS), is a tandem mass spectrometer consisting of two quadrupole mass analyzers in series, with a (non-mass-resolving) radio frequency (RF)–only quadrupole between them to act as a cell for collision-induced dissociation. This configuration is often abbreviated QqQ, here Q1q2Q3.

<span class="mw-page-title-main">Instrumental chemistry</span> Study of analytes using scientific instruments

Instrumental analysis is a field of analytical chemistry that investigates analytes using scientific instruments.

A liquid metal electrode is an electrode that uses a liquid metal, such as mercury, Galinstan, and NaK. They can be used in electrocapillarity, voltammetry, and impedance measurements.

References

  1. "Analytical technique". Archived from the original on 2013-03-17. Retrieved 2013-01-17.
  2. 1 2 3 Douglas A. Skoog; Stanley R. Crouch (2014). Fundamentals of analytical chemistry (Ninth ed.). Belmont, CA. ISBN   978-0-495-55828-6. OCLC   824171785.{{cite book}}: CS1 maint: location missing publisher (link)
  3. Skoog, Douglas A.; Donald M. West; F. James Holler (1996). Fundamentals of analytical chemistry (7th ed.). Fort Worth: Saunders College Pub. ISBN   0-03-005938-0. OCLC   33112372.
  4. Bard, Allen J.; Larry R. Faulkner (2001). Electrochemical methods : fundamentals and applications (Second ed.). Hoboken, NJ. ISBN   0-471-04372-9. OCLC   43859504.{{cite book}}: CS1 maint: location missing publisher (link)
  5. Poole, C. F. (2000-01-01), "CHROMATOGRAPHY", in Wilson, Ian D. (ed.), Encyclopedia of Separation Science, Oxford: Academic Press, pp. 40–64, ISBN   978-0-12-226770-3 , retrieved 2022-10-07