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A flame ionization detector (FID) is a scientific instrument that measures analytes in a gas stream. It is frequently used as a detector in gas chromatography. The measurement of ion per unit time make this a mass sensitive instrument.Standalone FIDs can also be used in applications such as landfill gas monitoring, fugitive emissions monitoring and internal combustion engine emissions measurement in stationary or portable instruments.
The first flame ionization detectors were developed simultaneously and independently in 1957 by McWilliam and Dewar at Imperial Chemical Industries of Australia and New Zealand (ICIANZ, see Orica history) Central Research Laboratory, Ascot Vale, Melbourne, Australia.and by Harley and Pretorius at the University of Pretoria in Pretoria, South Africa.
In 1959, Perkin Elmer Corp. included a flame ionization detector in its Vapor Fractometer.
The operation of the FID is based on the detection of ions formed during combustion of organic compounds in a hydrogen flame. The generation of these ions is proportional to the concentration of organic species in the sample gas stream.
To detect these ions, two electrodes are used to provide a potential difference. The positive electrode acts as the nozzle head where the flame is produced. The other, negative electrode is positioned above the flame. When first designed, the negative electrode was either tear-drop shaped or angular piece of platinum. Today, the design has been modified into a tubular electrode, commonly referred to as a collector plate. The ions thus are attracted to the collector plate and upon hitting the plate, induce a current. This current is measured with a high-impedance picoammeter and fed into an integrator. The manner in which the final data is displayed is based on the computer and software. In general, a graph is displayed that has time on the x-axis and total ion on the y-axis.
The current measured corresponds roughly to the proportion of reduced carbon atoms in the flame. Specifically how the ions are produced is not necessarily understood, but the response of the detector is determined by the number of carbon atoms (ions) hitting the detector per unit time. This makes the detector sensitive to the mass rather than the concentration, which is useful because the response of the detector is not greatly affected by changes in the carrier gas flow rate.
FID measurements are usually reported "as methane," meaning as the quantity of methane which would produce the same response. The same quantity of different chemicals produces different amounts of current, depending on the elemental composition of the chemicals. The response factor of the detector for different chemicals can be used to convert current measurements into actual amounts of each chemical.
Hydrocarbons generally have response factors that are equal to the number of carbon atoms in their molecule (more carbon atoms produce greater current), while oxygenates and other species that contain heteroatoms tend to have a lower response factor. Carbon monoxide and carbon dioxide are not detectable by FID.
FID measurements are often labelled "total hydrocarbons"or "total hydrocarbon content" (THC), although a more accurate name would be "total volatile hydrocarbon content" (TVHC), as hydrocarbons which have condensed out are not detected, even though they are important, for example safety when handling compressed oxygen.
The design of the flame ionization detector varies from manufacturer to manufacturer, but the principles are the same. Most commonly, the FID is attached to a gas chromatography system.
The eluent exits the gas chromatography column (A) and enters the FID detector’s oven (B). The oven is needed to make sure that as soon as the eluent exits the column, it does not come out of the gaseous phase and deposit on the interface between the column and FID. This deposition would result in loss of eluent and errors in detection. As the eluent travels up the FID, it is first mixed with the hydrogen fuel (C) and then with the oxidant (D). The eluent/fuel/oxidant mixture continues to travel up to the nozzle head where a positive bias voltage exists. This positive bias helps to repel the oxidized carbon ions created by the flame (E) pyrolyzing the eluent. The ions (F) are repelled up toward the collector plates (G) which are connected to a very sensitive ammeter, which detects the ions hitting the plates, then feeds that signal to an amplifier, integrator, and display system(H). The products of the flame are finally vented out of the detector through the exhaust port (J).
Flame ionization detectors are used very widely in gas chromatography because of a number of advantages.
Flame ionization detectors cannot detect inorganic substances and some highly oxygenated or functionalized species like infrared and laser technology can. In some systems, CO and CO2 can be detected in the FID using a methanizer, which is a bed of Ni catalyst that reduces CO and CO2 to methane, which can be in turn detected by the FID. The methanizer is limited by its inability to reduce compounds other than CO and CO2 and its tendency to be poisoned by a number of chemicals commonly found in gas chromatography effluents.
Another important disadvantage is that the FID flame oxidizes all oxidizable compounds that pass through it; all hydrocarbons and oxygenates are oxidized to carbon dioxide and water and other heteroatoms are oxidized according to thermodynamics. For this reason, FIDs tend to be the last in a detector train and also cannot be used for preparatory work.
An improvement to the methanizer is the Polyarc reactor, which is a sequential reactor that oxidizes compounds before reducing them to methane. This method can be used to improve the response of the FID and allow for the detection of many more carbon-containing compounds.The complete conversion of compounds to methane and the now equivalent response in the detector also eliminates the need for calibrations and standards because response factors are all equivalent to those of methane. This allows for the rapid analysis of complex mixtures that contain molecules where standards are not available.
Mass spectrometry (MS) is an analytical technique that is used to measure the mass-to-charge ratio of ions. The results are presented as a mass spectrum, a plot of intensity as a function of the mass-to-charge ratio. Mass spectrometry is used in many different fields and is applied to pure samples as well as complex mixtures.
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.
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.
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, 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.
The proportional counter is a type of gaseous ionization detector device used to measure particles of ionizing radiation. The key feature is its ability to measure the energy of incident radiation, by producing a detector output pulse that is proportional to the radiation energy absorbed by the detector due to an ionizing event; hence the detector's name. It is widely used where energy levels of incident radiation must be known, such as in the discrimination between alpha and beta particles, or accurate measurement of X-ray radiation dose.
Chemical ionization (CI) is a soft ionization technique used in mass spectrometry. This was first introduced by Burnaby Munson and Frank H. Field in 1966. This technique is a branch of gaseous ion-molecule chemistry. Reagent gas molecules are ionized by electron ionization, which subsequently react with analyte molecules in the gas phase in order to achieve ionization. Negative chemical ionization (NCI), charge-exchange chemical ionization and atmospheric-pressure chemical ionization (APCI), atmospheric pressure photoionization (APPI) are some of the common variations of this technique. CI has several important applications in identification, structure elucidation and quantitation of organic compounds. Beside the applications in analytical chemistry, the usefulness in chemical ionization extends toward biochemical, biological and medicinal fields as well.
Gaseous ionization detectors are radiation detection instruments used in particle physics to detect the presence of ionizing particles, and in radiation protection applications to measure ionizing radiation.
An electron capture detector (ECD) is a device for detecting atoms and molecules in a gas through the attachment of electrons via electron capture ionization. The device was invented in 1957 by James Lovelock and is used in gas chromatography to detect trace amounts of chemical compounds in a sample.
A photoionization detector or PID is a type of gas detector.
A gas detector is a device that detects the presence of gases in an area, often as part of a safety system. A gas detector can sound an alarm to operators in the area where the leak is occurring, giving them the opportunity to leave. This type of device is important because there are many gases that can be harmful to organic life, such as humans or animals.
The thermal conductivity detector (TCD), also known as a katharometer, is a bulk property detector and a chemical specific detector commonly used in gas chromatography. This detector senses changes in the thermal conductivity of the column eluent and compares it to a reference flow of carrier gas. Since most compounds have a thermal conductivity much less than that of the common carrier gases of helium or hydrogen, when an analyte elutes from the column the effluent thermal conductivity is reduced, and a detectable signal is produced.
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Electron capture ionization is the ionization of a gas phase atom or molecule by attachment of an electron to create an ion of the form . The reaction is
A chromatography detector is a device used in gas chromatography (GC) or liquid chromatography (LC) to detect components of the mixture being eluted off the chromatography column. There are two general types of detectors: destructive and non-destructive. The destructive detectors perform continuous transformation of the column effluent with subsequent measurement of some physical property of the resulting material. The non-destructive detectors are directly measuring some property of the column eluent and thus affords greater analyte recovery.
Amperometry in chemistry is detection of ions in a solution based on electric current or changes in electric current.
Methanizer is an appliance used in gas chromatography (GC), which allows the user to detect very low concentrations of carbon monoxide and carbon dioxide. It consists of a flame ionization detector, preceded by a hydrogenating reactor, which converts CO2 and CO into methane CH4. Methanizers contain a hydrogenation catalyst to achieve this conversion. Nickel is commonly used as the catalyst and there are alternatives available.
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The Charged Aerosol Detector (CAD) is a detector used in conjunction with high-performance liquid chromatography (HPLC) and ultra high-performance liquid chromatography (UHPLC) to measure the amount of chemicals in a sample by creating charged aerosol particles which are detected using an electrometer. It is commonly used for the analysis of compounds that cannot be detected using traditional UV/Vis approaches due to their lack of a chromophore. The CAD can measure all non-volatile and many semi-volatile analytes including, but not limited to, antibiotics, excipients, ions, lipids, natural products, biofuels, sugars and surfactants. The CAD, like other aerosol detectors, falls under the category of destructive general-purpose detectors.
The Polyarc reactor is a scientific instrument for the measurement of organic molecules. The reactor is paired with a flame ionization detector (FID) in a gas chromatograph (GC) to improve the sensitivity of the FID and give a uniform detector response for all organic molecules (GC-Polyarc/FID).
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