Analytical techniques gas chromatography

Stage II Sequential analytical techniques Gas chromatography Gas chromatography coupled with mass spectrometry, multidimensional gas chromatography... 

The isolation of atropine, scopolamine, and cocaine occurred long before the development of modern analytical techniques. Gas chromatography was the first instrumental technique available in the field of separation science and thus it is not surprising that these alkaloids were firstly analyzed by GC despite their low volatility. With the advent of capillary columns and the proliferation of various sample introduction and detection methods, GC has evolved as the dominant analytical technique for screening, identification, and quantitation of tropane alkaloids of plant origin as well as in biological fluids. The state-of-the-art of GC analysis of tropane alkaloids has been the subject of two comprehensive reviews [45,58]. We shall therefore mainly focus on publications which have appeared since 2002. 

Although best known as an analytical technique, gas chromatography is also used to make physical measurements (JL). Applications to polymeric substrates where the material under study is the stationary phase in the GC column have been reviewed (2, 3.). 

Infrared spectroscopy has been. combined with various other analytical techniques. Gas chromatography-infrared spectroscopy (GC-IR) allows the identification of the components eluting froiti a gas chromatograph. GC-IR has certain advantages over, say, gas chromatography-mass spectrometry (GC-MS). While GC-MS is able to distinguish easily between compounds of different mass, it is unable to differentiate structural isomers of the same molecular mass. By comparison, GC-IR can easily distinguish such isomers. 

Gas chromatography. See Analytical techniques Gas Safety (Installation and Use) Regulations 1994, 595 Gas Safety (Management) Regulations 1996, 484 Gases, See also Asphyxiants Compressed gases definition, 26... 

The flavor impression of a food is influenced by compounds that affect both taste and odor. The analysis and identification of many volatile flavor compounds in a large variety of food products have been assisted by the development of powerful analytical techniques. Gas-liquid chromatography was widely used in the early 1950s when commercial instruments became available. Introduction of the flame ionization detector increased sensitivity by a factor of 100 and, together with mass spectrometers, gave a method for rapid identification of many components in complex mixtures. These methods have been described by Teranishi et al. (1971). As a result, a great deal of information on volatile flavor components has been obtained in recent years for a variety of food products. The combination of gas chromatography and mass spectrometry can provide identification and quantitation of flavor compounds. However, when the flavor consists of many compounds, sometimes several hun-... 

A suitable technique for this purpose (concentration of trace components and their isolation in a new reaction) involves the use of a liquid bubbler. The applicability of this technique in analytical reaction gas chromatography was shown earlier [15] using as an example the preliminary concentration of hydrogen sulphide and carbon dioxide by means of an alkaline solution of sodium hydroxide through which a flow of the sample gas was passed. When the solution was acidified, the acidic traces formed a concentrated zone, and were separated on a chromatographic column. A liquid bubbler as illustrated in Fig. 8.3 was used to concentrate the trace components. 

See also Clinical Analysis Sample Handling. Derivatization of Analytes. Forensic Sciences Systematic Drug Identification Thin-Layer Chromatography. Fourier Transform Techniques. Gas Chromatography Mass Spectrometry Forensic Applications. Immunoassays, Applications Clinical Forensic. Liquid Chromatography Normal Phase Reversed Phase. Spectrophotometry Pharmaceutical Applications. 

To establish the mechanism of thermal decomposition of organically modified layered silicates, various analytical and thermoanalytical methods have been applied, including thermogravimetric analysis (TGA), pyrolysis techniques, gas chromatography (GC), and mass spectrometry (MS) [12,15,17,18]. 

Analytical separations may be classified in three ways by the physical state of the mobile phase and stationary phase by the method of contact between the mobile phase and stationary phase or by the chemical or physical mechanism responsible for separating the sample s constituents. The mobile phase is usually a liquid or a gas, and the stationary phase, when present, is a solid or a liquid film coated on a solid surface. Chromatographic techniques are often named by listing the type of mobile phase, followed by the type of stationary phase. Thus, in gas-liquid chromatography the mobile phase is a gas and the stationary phase is a liquid. If only one phase is indicated, as in gas chromatography, it is assumed to be the mobile phase. 

Gas chromatography/ma.ss spectrometry (GC/MS) is an analytical technique combining the advantages of a GC instrument with those of a mass spectrometer. 

Methods for iodine deterrnination in foods using colorimetry (95,96), ion-selective electrodes (94,97), micro acid digestion methods (98), and gas chromatography (99) suffer some limitations such as potential interferences, possibHity of contamination, and loss during analysis. More recendy neutron activation analysis, which is probably the most sensitive analytical technique for determining iodine, has also been used (100—102). 

Air Monitoring. The atmosphere in work areas is monitored for worker safety. Volatile amines and related compounds can be detected at low concentrations in the air by a number of methods. Suitable methods include chemical, chromatographic, and spectroscopic techniques. For example, the NIOSH Manual of Analytical Methods has methods based on gas chromatography which are suitable for common aromatic and aHphatic amines as well as ethanolamines (67). Aromatic amines which diazotize readily can also be detected photometrically using a treated paper which changes color (68). Other methods based on infrared spectroscopy (69) and mass spectroscopy (70) have also been reported. 

There are a variety of analytical methods commonly used for the characterization of neat soap and bar soaps. Many of these methods have been pubUshed as official methods by the American Oil Chemists Society (29). Additionally, many analysts choose United States Pharmacopoeia (USP), British Pharmacopoeia (BP), or Pood Chemical Codex (FCC) methods. These methods tend to be colorimetric, potentiometric, or titrametric procedures. However, a variety of instmmental techniques are also frequendy utilized, eg, gas chromatography, high performance Hquid chromatography, nuclear magnetic resonance spectroscopy, infrared spectroscopy, and mass spectrometry. 

Analytical Techniques. Sorbic acid and potassium sorbate are assayed titrimetricaHy (51). The quantitative analysis of sorbic acid in food or beverages, which may require solvent extraction or steam distillation (52,53), employs various techniques. The two classical methods are both spectrophotometric (54—56). In the ultraviolet method, the prepared sample is acidified and the sorbic acid is measured at 250 260 nm. In the colorimetric method, the sorbic acid in the prepared sample is oxidized and then reacts with thiobarbituric acid the complex is measured at - 530 nm. Chromatographic techniques are also used for the analysis of sorbic acid. High pressure Hquid chromatography with ultraviolet detection is used to separate and quantify sorbic acid from other ultraviolet-absorbing species (57—59). Sorbic acid in food extracts is deterrnined by gas chromatography with flame ionization detection (60—62). 

Mixtures can be identified with the help of computer software that subtracts the spectra of pure compounds from that of the sample. For complex mixtures, fractionation may be needed as part of the analysis. Commercial instmments are available that combine ftir, as a detector, with a separation technique such as gas chromatography (gc), high performance Hquid chromatography (hplc), or supercritical fluid chromatography (96,97). Instmments such as gc/ftir are often termed hyphenated instmments (98). Pyrolyzer (99) and thermogravimetric analysis (tga) instmmentation can also be combined with ftir for monitoring pyrolysis and oxidation processes (100) (see Analytical methods, hyphenated instruments). 

Purity of toluene samples as well as the number, concentration, and identity of other components can be readily determined using standard gas chromatography techniques (40—42). Toluene content of high purity samples can also be accurately measured by freezing point, as outlined in ASTM D1016. Toluene exhibits characteristic uv, it, nmr, and mass spectra, which are useful in many specific control and analytical problems (2,43—45). 

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