Functional groups analytical determination

More recently, the same author [41] has described polymer analysis (polymer microstructure, copolymer composition, molecular weight distribution, functional groups, fractionation) together with polymer/additive analysis (separation of polymer and additives, identification of additives, volatiles and catalyst residues) the monograph provides a single source of information on polymer/additive analysis techniques up to 1980. Crompton described practical analytical methods for the determination of classes of additives (by functionality antioxidants, stabilisers, antiozonants, plasticisers, pigments, flame retardants, accelerators, etc.). Mitchell... 

Selection of columns and mobile phases is determined after consideration of the chemistry of the analytes. In HPLC, the mobile phase is a liquid, while the stationary phase can be a solid or a liquid immobilised on a solid. A stationary phase may have chemical functional groups or compounds physically or chemically bonded to its surface. Resolution and efficiency of HPLC are closely associated with the active surface area of the materials used as stationary phase. Generally, the efficiency of a column increases with decreasing particle size, but back-pressure and mobile phase viscosity increase simultaneously. Selection of the stationary phase material is generally not difficult when the retention mechanism of the intended separation is understood. The fundamental behaviour of stationary phase materials is related to their solubility-interaction... 

Advances have been achieved in recent years, such as the use of CL reagents as labels to derivatize and sensitively determine analytes containing amine, carboxyl, hydroxy, thiol, and other functional groups and their application in HPLC and CE [35, 36], the synthesis and application of new acridinium esters [37], the development of enhanced CL detection of horseradish peroxidase (HRP) labels [38], the use of immobilization techniques for developing CL-based sensors [39-42], some developments of luminol-based CL in relation to its application to time-resolved or solid-surface analysis [43], and the analytical application of electrogenerated CL (ECL) [44-47], among others. 

When an examination is restricted to the identification of one or more constituents of a sample, it is known as qualitative analysis, while an examination to determine how much of a particular species is present constitutes a quantitative analysis. Sometimes information concerning the spatial arrangement of atoms in a molecule or crystalline compound is required or confirmation of the presence or position of certain organic functional groups is sought. Such examinations are described as structural analysis and they may be considered as more detailed forms of analysis. Any species that are the subjects of either qualitative or quantitative analysis are known as analytes. 

Most of the continuously monitored water contaminants are determined via gas chromatography-mass spectrometry (GC-MS). However, an adequate separation of polar compounds via GC typically requires derivatization of the polar moieties (e.g., BSTFA derivatives). In addition to this, as the analyte groups show different properties concerning the number and kind of functional groups, it is quite difficult to develop a universal derivatization procedure suitable for all the target analytes. Furthermore, the presence in wastewater of many other organic compounds requires the use of labeled standards, which can make application of this method unfeasible [35]. 

There are certain rules determining fragmentation of organic compounds in a mass spectrometer. That is why on the basis of the fragmentation pattern it is possible to define the molecular mass, elemental composition, presence of certain functional groups, and often the structure of an analyte. There are a lot of similarities in the mass spectrometric behavior of related compounds. This fact facilitates manual interpretation of a mass spectrum, although it requires some experience. It is also worth mentioning that mass... 

The determination of endogenous compounds and drugs in biological matrices has always presented a formidable challenge as one has to consider various factors before attempting to develop a suitable HPLC assay. These include the physicochemical properties of the compound such as the pKa value, solubility, volatility, particular functional groups (e.g., possessing chromophores, fluorophores, or electroactive characteristics), potential metabolites, and the required sensitivity and specificity. All these aspects will determine the type of extraction processes, analytical column selection, and suitable detector systems to be used as part of the HPLC apparatus. 

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