Solid phase, partitioning with

The proposed proeedure are detailed next eaeh SPMD was mierowave-assisted extraeted twiee with 30 mL hexane aeetone, and irradiated with 250 W power output, until 90°C in 10 minutes, being this temperature held for another 10 minutes. Clean-up of extraet was performed by aeetonitrile-hexane partitioning eoupled by a solid-phase extraetion with a eombined eartridge of 2 g basie-alumina (deaetivated with 5% water) and 0.5 g C. ... 

Nakamura, M., Suzuki, T., Amano, K., and Yamada, S. Relation of sorption behavior of agricultural chemicals in solid-phase extraction with their n-octanolAvater partition coefficients evaluated by high-performance liquid chromatography. Anal Chim. Acta, 428(2) 219-226, 2001. 

Takeuchi, Curran, and co-workers synthesized a fluorous chiral diol, (R)-2,2 bis[(S)-2-hydroxy-2-phenylethoxy]-6,6 -bis[tris(lH,lH,2H,2H-perfluorooctyl)silyl]-l,T-binaphthyl ((R,S)-FDHPEB) (F content = 56%, partition coefficient benzene/ FC-72 = 1 32, THF/FC-72 = 19 1) and applied it to a Sml2-mediated enantio-selective protonation of 2-methoxy-2-phenylcyclohexanone [2], The reaction was carried out under the same reaction conditions as those of the original nonfluorous reaction [3], In the original reaction, the product was separated from the nonfluorous chiral proton source (2 equiv realtive to the substrate) with preparative TLC to give the product in 70% chemical yield and 87% ee. In the fluorous version, the product and the fluorous chiral proton source were separated by FC-72 extraction (six times) and more simply by fluorous solid-phase extraction with an FRP silica gel column. 

A recent method, still in development, for determining total 4-nitrophenol in the urine of persons exposed to methyl parathion is based on solid phase microextraction (SPME) and GC/MS previously, the method has been used in the analysis of food and environmental samples (Guidotti et al. 1999). The method uses a solid phase microextraction fiber, is inserted into the urine sample that has been hydrolyzed with HCl at 50° C prior to mixing with distilled water and NaCl and then stirred (1,000 rpm). The fiber is left in the liquid for 30 minutes until a partitioning equilibrium is achieved, and then placed into the GC injector port to desorb. The method shows promise for use in determining exposures at low doses, as it is very sensitive. There is a need for additional development of this method, as the measurement of acetylcholinesterase, the enzyme inhibited by exposure to organophosphates such as methyl parathion, is not an effective indicator of low-dose exposures. 

Solid phase micro extraction (SPME) is a techniques in which a silica fiber coated with a thin film of polymer is brought into contact with an aqueous matrix where the organics in solution partition onto the fiber. The fiber is subsequently placed into the injector of a GC where the heat causes the release of analyte onto the column. This has been applied to endosulfan (a- and (3-) and endosulfan sulfate in water with limits of detection of less than 0.3 pg/L reported (Magdic and Pawliszyn 1996). 

Deposition of adamantane from petroleum streams is associated with phase transitions resulting from changes in temperature, pressure, and/or composition of reservoir fluid. Generally, these phase transitions result in a solid phase from a gas or a liquid petroleum fluid. Deposition problems are particularly cumbersome when the fluid stream is dry (i.e., low LPG content in the stream). Phase segregation of solids takes place when the fluid is cooled and/or depressurized. In a wet reservoir fluid (i.e., high LPG content in the stream) the diamondoids partition into the LPG-rich phase and the gas phase. Deposition of diamondoids from a wet reservoir fluid is not as problematic as in the case of dry streams [74, 75]. 

Analytical methods for parent chloroacetanilide herbicides in soil typically involve extraction of the soil with solvent, followed by solid-phase extraction (SPE), and analysis by gas chromatography/electron capture detection (GC/ECD) or gas chromatog-raphy/mass spectrometry (GC/MS). Analytical methods for parent chloroacetanilides in water are similarly based on extraction followed by GC with various detection techniques. Many of the water methods, such as the Environmental Protection Agency (EPA) official methods, are multi-residue methods that include other compound classes in addition to chloroacetanilides. While liquid-liquid partitioning was used initially to extract acetanilides from water samples, SPE using... 

A soil sample (10 g) was extracted by mechanically shaking with methanol-deionized water. This mixture was filtered and a portion was removed for partitioning into toluene-hexane. A phenyl solid-phase extraction (SPE) cartridge was employed... 

For the analysis of organic additives in polymeric materials, in most cases, prior extraction will be necessary. Depending on the nature of the additive, many different approaches are employed. These include soxhlet extraction with organic solvent or aqueous media, total sample dissolution followed by selective precipitation of the polymer leaving the additive in solution, assisted extraction using pressurised systems, ultrasonic agitation and the use of supercritical fluids. In trace analysis, solid phase extraction (SPME) from solution or solvent partition may be required to increase the analyte concentration. 

Partition coefficient between octanol and air (K0A) is determined by the relationship of chemical concentrations in octanol and air (K0a = Co/CA). The K0A is directly connected with the soil-air partition coefficient of pollutant K A which is determined as the ratio of solid phase to air concentrations (Ksa = Cs/CA) or through other constants (KSA = KSw/KAw). 

Solid-phase microextraction (SPME) is also a useful alternative to conventional sample cleanup with LLE or SPE. SPME is based on the enrichment of analytes by a partitioning process between a polymeric phase coated on a fused-silica fiber and its surrounding aqueous solution. SPME combines sample preparation in terms of extraction from a matrix of interfering compounds with an enrichment process in a single step. A method for the determination of metazachlor in wastewater samples is described in the literature [34]. In this study, SPME was shown to be a suitable and simple sample preparation method for the determination of metazachlor in wastewater by GC-AED. 

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