Extractants organic phase composition

Nilsson, M. Influence of Organic Phase Composition on the Extraction ofTrivalent Actinides, Dipl, work. Dept. Nucl. Chem., Chalmers Univ. of Techn., Gothenburg, 2000. 

Figure 8 Effect of anion type on the extraction efficiency of four copper salts as a function of ligand concentration (organic phase composition 0.5 M TOA + 0.5 M 2-ethylhexanoic acid in toluene).

Relationships connecting stmcture and properties of primary alkylamines of normal stmcture C, -C gin chloroform and other solvents with their ability to extract Rh(III) and Ru(III) HCA from chloride solutions have been studied. The out-sphere mechanism of extraction and composition of extracted associates has been ascertained by UV-VIS-, IR-, and H-NMR spectroscopy, saturation method, and analysis of organic phase. Tertiary alkylamines i.e. tri-n-octylamine, tribenzylamine do not extract Ru(III) and Rh(III) HCA. The decrease of radical volume of tertiary alkylamines by changing of two alkyl radicals to methyl make it possible to diminish steric effects and to use tertiary alkylamines with different radicals such as dimethyl-n-dodecylamine which has not been used previously for the extraction of Rh(III), Ru(III) HCA with localized charge. 

The effect of the variation in mobile phase composition can be overcome by the use of post-column on-line extraction to remove water from the mobile phase and thus produce a 100% organic mobile phase and this is also likely to bring about an increase in overall sensitivity. 

A similar study has been carried out in order to test the capacity of RP-HPLC for the authenticity test of chilli powders on the basis of pigment composition. Carotenoid pigments were extracted by shaking 3 g of chilli powder with 10 ml of acetone for 30 min. The supernatant was decanted and the procedure was repeated as the solid rest was nearly colourless. The collected organic phases were evaporated and redissolved in the mobile phase. Separations were performed on a narrow-bore ODS column (150 X 2 mm i.d., carbon loading, 9.5 per cent). Eluents A and B were methanol-ACN (80 20, v/v) and bidistilled water, respectively. Gradient elution was initiated by 15 per cent A increased to 80 per cent A in 25 min, held for 10 min, increased to 90 per cent A in 10 min, held for 10 min, increased to 97 per cent A in 3 min and held for 62 min. Each step of gradient elution was linear. Measurements were... 

Another study employed an ODS column and different mobile phase composition for the measurement of carotenoids in orange juice. Citrus fruits were hand-squeezed and the juice was filtered. Aliquots of 5 ml of juice were extracted with ethyl acetate (3 X 50 ml) containing 0.004 per cent butyl hydroxytoluene (BHT). The organic phase was dried with 50 g of anhydrous sodium sulphate and the aqueous phase was mixed with 50 ml of mehanol and 100 ml of 1 M NaCl, extracted with 75 and 25 ml of ethyl acetate. The ethyl acetate fractions were combined, evaporated to dryness at 40°C and redissolved in the mobile phase. Extracts were analysed in an ODS column (250 X 4.6 mm i.d. particle size 5 jian). The mobile phase consisted of ACN-methanol-l,2-dichloroethane (60 35 5, v/v) containing 0.1 per cent BHT, 0.1 per cent triethylamine and 0.05 M of ammonium acetate. The column was not thermostated and the flow rate was 1 ml/min. Pigments were detected... 

Various liquid chromatographic techniques have been frequently employed for the purification of commercial dyes for theoretical studies or for the exact determination of their toxicity and environmental pollution capacity. Thus, several sulphonated azo dyes were purified by using reversed-phase preparative HPLC. The chemical strctures, colour index names and numbers, and molecular masses of the sulphonated azo dyes included in the experiments are listed in Fig. 3.114. In order to determine the non-sulphonated azo dyes impurities, commercial dye samples were extracted with hexane, chloroform and ethyl acetate. Colourization of the organic phase indicated impurities. TLC carried out on silica and ODS stationary phases was also applied to control impurities. Mobile phases were composed of methanol, chloroform, acetone, ACN, 2-propanol, water and 0.1 M sodium sulphate depending on the type of stationary phase. Two ODS columns were employed for the analytical separation of dyes. The parameters of the columns were 150 X 3.9 mm i.d. particle size 4 /jm and 250 X 4.6 mm i.d. particle size 5 //m. Mobile phases consisted of methanol and 0.05 M aqueous ammonium acetate in various volume ratios. The flow rate was 0.9 ml/min and dyes were detected at 254 nm. Preparative separations were carried out in an ODS column (250 X 21.2 mm i.d.) using a flow rate of 13.5 ml/min. The composition of the mobile phases employed for the analytical and preparative separation of dyes is compiled in Table 3.33. 

Since most APIs have some aqueous solubility, extraction is typically performed at room temperature with aqueous or a mixture of aqueous and organic media.Extraction can be performed in one step with a single solvent or in multiple steps executed sequentially with different solvents. The extraction solvent must be able to solubilize the API and be compatible with the HPLC mobile phase for the final analysis. The pH, buffer concentration and organic solvent composition of the extraction... 

Further improvement of the synthetic performance of the reaction system was attempted by adapting the composition of the organic phase in such a way that partition of products into the organic phase was enhanced. In the synthesis of (R) -3,3 -furoin, product extraction was increased by 11% when hexane was mixed with 2-octanone in a ratio of 3 1, while replacing hexane with pure 2-octanone, 2-pentanone, 2-butanone, heptane, or decane yielded considerably lower product concentrations. No apparent rule was underlying these results. 

The robustness of an analytical procedure is a measure of its capacity to remain unaffected by small but deliberate variations in the analytical procedure parameters. The robustness of the analytical procedure provides an indication of its reliability during normal use. The evaluation of robustness should be considered during development of the analytical procedure. If measurements are susceptible to variations in analytical conditions, the analytical conditions should be suitably controlled or a precautionary statement should be included in the procedure. For example, if the resolution of a critical pair of peaks was very sensitive to the percentage of organic composition in the mobile phase, that observation would have been observed during method development and should be stressed in the procedure. Common variations that are investigated for robustness include filter effect, stability of analytical solutions, extraction time during sample preparation, pH variations in the mobile-phase composition, variations in mobile-phase composition, columns, temperature effect, and flow rate. 

Figure 6. Absorption spectra of the components in the organic phase obtained after extraction of photogenerated CgV+ from the aqueous phase a) Composite spectrum of CgV+ and CgV in ethylacetate after illumination of the system for 10 minutes b) Spectrum of CgV in ethylaaetate obtained after subtraction of CgV+.spectrum from the composite spectrum (a). Insert is enlarged absorption spectrum of CgV. c) Spectrum of the photoproducts when toluene is used as the organic phase in the two phase system. Spectrum recorded after illumination for 15 minutes corresponds to CgV as major product.

Another method for obtaining the extension domain of the organic extractant phase before third-phase formation is to prepare a solution under the conditions of formation of a third phase, and allow it to equilibrate. Chemical analysis of the third phase and the dilute organic phase in equilibrium with the aqueous phase identifies tie-lines in the phase diagrams (Figure 7.5) (a tie-line joins the composition of the two phases (dilute and concentrated) in equilibrium after the splitting of the organic phase into two phases). 

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