Thin solvent extraction

The liquid-liquid interface is not only a boundary plane dividing two immiscible liquid phases, but also a nanoscaled, very thin liquid layer where properties such as cohesive energy, density, electrical potential, dielectric constant, and viscosity are drastically changed along with the axis from one phase to another. The interfacial region was anticipated to cause various specific chemical phenomena not found in bulk liquid phases. The chemical reactions at liquid-liquid interfaces have traditionally been less understood than those at liquid-solid or gas-liquid interfaces, much less than the bulk phases. These circumstances were mainly due to the lack of experimental methods which could measure the amount of adsorbed chemical species and the rate of chemical reaction at the interface [1,2]. Several experimental methods have recently been invented in the field of solvent extraction [3], which have made a significant breakthrough in the study of interfacial reactions. 

The introduction of a third phase - the membrane phase - between the two conventional phases (i.e., the aqueous and the organic phases) helps in overcoming many of the problems of solvent extraction. The membrane phase is a thin film, immiscible with the aque-... 

Polymer/additive analysis then usually proceeds by separation of polymer and additives (cf. Scheme 2.12) using one out of many solvent extraction techniques (cf. Chapter 3). After extraction the residue is pressed into a thin film to verify that all extractables have been removed. UV spectroscopy is used for verification of the presence of components with a chromophoric moiety (phenolic antioxidants and/or UV absorbers) and IR spectroscopy to verify the absence of IR bands extraneous to the polymer. The XRF results before and after extraction are compared, especially when the elemental analysis does not comply with the preliminary indications of the nature of the additive package. This may occur for example in PA6/PA6.6 blends where... 

The conventional approach to solvent extraction is the batch method. Early work with this method was hampered by the low concentration of the compounds present and the relative insensitivity of the methods of characterization. Thus lipids and hydrocarbons have been separated from seawater by extraction with petroleum ether and ethyl acetate. The fractionation techniques include column and thin-layer chromatography with final characterisation by thin-layer chromatography, infrared, and ultra-violet spectroscopy and gas chromatography. Of these techniques, only gas chromatography is really useful at levels of organic matter present in seawater. With techniques available today such as glass capillary gas chromatography and mass spectrometry, much more information could be extracted from such samples [20]. 

Thin layer chromatography of the solvent extracts was carried out on Whatman LKSDF silica gel 250pm plates. The plates were developed in ascending fashion with 1 1 1 hexane acetone toluene or hexane. After drying, the lanes were divided into 1cm sections and the silica gel recovered for counting of the labelled benzo[a]pyrene and anthracene. 

The formulation of the three phases must be such that the liquid membrane extracts the solute from one of the phases and the third phase strips it from the membrane. Thus extraction and stripping take place in the same contactor, and the stripping phase is where the solute is accumulated, instead of the organic phase as in the case of conventional solvent extraction. This allows for a middle phase of small volume that, being thin, behaves like a membrane. 

Colloidal liquid aphrons (CLAs), obtained by diluting a polyaphron phase, are postulated to consist of a solvent droplet encapsulated in a thin aqueous film ( soapy-shell ), a structure that is stabilized by the presence of a mixture of nonionic and ionic surfactants [57]. Since Sebba s original reports on biliquid foams [58] and subsequently minute oil droplets encapsulated in a water film [59], these structures have been investigated for use in predispersed solvent extraction (PDSE) processes. Because of a favorable partition coefficient for nonpolar solutes between the oil core of the CLA and a dilute aqueous solution, aphrons have been successfully applied to the extraction of antibiotics [60] and organic pollutants such as dichlorobenzene [61] and 3,4-dichloroaniline [62]. 

Figure 1. Autoradiograc of thin layer chromatograErfiy plate showing solvent extractable naphthalene metabolites (A, B, C, D) produced by transformants Nah 1, Nah 25, Nah 28, B. megaterium, and B. subtilis. ...

The method of solvent extraction/liquid chromatography analysis of relatively large and thin samples (10 — 15 fim layer on a glass disc with a diameter of 40 mm, sample weight 15 — 20 mg) has been described in a previous publication (14). 

Many [M(dik)4] complexes are volatile, especially those that contain fluorinated diketonate ligands. Mass spectra and gas chromatographic behavior of several of these complexes have been studied (see Table 10). Isenhour and coworkers240 241 have employed fluorinated diketonates in mass spectrometric procedures for determination of Zr and Zr/Hf ratios in geological samples. The most intense peak in mass spectra of [M(dik)4] complexes is [M(dik)3]+. Sievers et al.242 have used gas chromatography of metal trifluoroacetylacetonates to separate Zr from Al, Cr and Rh. However, attempts to separate [Zr(tfacac)4] and [Hf(tfacac)4] by gas chromatography were unsuccessful. Zirconium and hafnium can be separated by solvent extraction procedures that employ fluorinated diketones.105 [M(dik)4] (M = Zr or Hf dik = acac, dpm, tfacac or hfacac) have been used as volatile source materials for chemical vapor deposition of thin films of the metal oxides.243,244... 

Thin layer chromatographic Various adsorbent materials Water boundary layer Organophosphates Screening 1 month Solvent extraction 75... 

---