Chromatographic methods chromatography

Among the most precise and often applied analytical methods are various chromatographic methods. Chromatography is popular partly for its low cost, but also for its sensitivity, particularly when it is applied with a preconcentration separation that isolates the lanthanides from matrix elements. The most demanding analytical methods combine chromatographic techniques with element/isotope specific techniques like NAA or mass spectrometry (MS). The separation chemistry of the lanthanides and Y as a group and of individual members of the series, is the subject of this review. 

Table 4 lists the specifications set by Du Pont, the largest U.S. producer of DMF (4). Water in DMF is deterrnined either by Kad Fischer titration or by gas chromatography. The chromatographic method is more rehable at lower levels of water (<500 ppm) (4). DMF purity is deterrnined by gc. For specialized laboratory appHcations, conductivity measurements have been used as an indication of purity (27). DMF in water can be measured by refractive index, hydrolysis to DMA followed by titration of the Hberated amine, or, most conveniendy, by infrared analysis. A band at 1087 cm is used for the ir analysis. 

A review pubHshed ia 1984 (79) discusses some of the methods employed for the determination of phenytoia ia biological fluids, including thermal methods, spectrophotometry, luminescence techniques, polarography, immunoassay, and chromatographic methods. More recent and sophisticated approaches iaclude positive and negative ion mass spectrometry (80), combiaed gas chromatography—mass spectrometry (81), and ftir immunoassay (82). 

To determine the phosphoHpid and fatty acid compositions chromatographic methods (28) like gas chromatography (gc), thin-layer chromatography (tic), and high performance Hquid chromatography (hlpc) are used. Newer methods for quantitative deterrnination of different phosphoHpid classes include P-nmr (29). 

Analytical and Test Methods. o-Nitrotoluene can be analyzed for purity and isomer content by infrared spectroscopy with an accuracy of about 1%. -Nitrotoluene content can be estimated by the decomposition of the isomeric toluene diazonium chlorides because the ortho and meta isomers decompose more readily than the para isomer. A colorimetric method for determining the content of the various isomers is based on the color which forms when the mononitrotoluenes are dissolved in sulfuric acid (45). From the absorption of the sulfuric acid solution at 436 and 305 nm, the ortho and para isomer content can be deterrnined, and the meta isomer can be obtained by difference. However, this and other colorimetric methods are subject to possible interferences from other aromatic nitro compounds. A titrimetric method, based on the reduction of the nitro group with titanium(III) sulfate or chloride, can be used to determine mononitrotoluenes (32). Chromatographic methods, eg, gas chromatography or high pressure Hquid chromatography, are well suited for the deterrnination of mononitrotoluenes as well as its individual isomers. Freezing points are used commonly as indicators of purity of the various isomers. 

Chromatographic Method. Progress in the development of chromatographic techniques (55), especially, in high performance Hquid chromatography, or hplc, is remarkable (56). Today, chiral separations are mainly carried out by three hplc methods chiral hplc columns, achiral hplc columns together with chiral mobile phases, and derivatization with optical reagents and separation on achiral columns. All three methods are usehil but none provides universal appHcation. 

Chromatographic methods, notably hplc, are available for the simultaneous deterrnination of ascorbic acid as weU as dehydroascorbic acid. Some of these methods result in the separation of ascorbic acid from its isomers, eg, erythorbic acid and oxidation products such as diketogulonic acid. Detection has been by fluorescence, uv absorption, or electrochemical methods (83—85). Polarographic methods have been used because of their accuracy and their ease of operation. Ion exclusion (86) and ion suppression (87) chromatography methods have recently been reported. Other methods for ascorbic acid deterrnination include enzymatic, spectroscopic, paper, thin layer, and gas chromatographic methods. ExceUent reviews of these methods have been pubHshed (73,88,89). 

For selective estimation of phenols pollution of environment such chromatographic methods as gas chromatography with flame-ionization detector (ISO method 8165) and high performance liquid chromatography with UV-detector (EPA method 625) is recommended. For determination of phenol, cresols, chlorophenols in environmental samples application of HPLC with amperometric detector is perspective. Phenols and chlorophenols can be easy oxidized and determined with high sensitivity on carbon-glass electrode. 

P. Sandra (Ed.), Sample Introduction in Capillary Gas Chromatography, Vol 1, Chromatographic Method Series, Huethig, Basel, 1985. 

Often, planar chromatography is used as a preparative step for the isolation of single components or classes of components for further chromatographic separation or spectroscopic elucidation. Many planar chromatographic methods have been developed for the analysis of food products, bioactive compounds from plant materials, and essential oils. 

Multidimensional chromatography has important applications in environmental analysis. Environmental samples may be very complex, and the fact that the range of polarity of the components is very wide, and that there are a good many isomers or congeners with similar or identical retention characteristics, does not allow their separation by using just one chromatographic method. 

Despite the difficulties caused by the rapidly expanding literature, the use of chiral stationary phases (CSPs) as the method of choice for analysis or preparation of enantiomers is today well established and has become almost routine. It results from the development of chiral chromatographic methods that more than 1000 chiral stationary phases exemplified by several thousands of enantiomer separations have been described for high-performance liquid chromatography (HPLC). 

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