Extraction fractional

Fractional extraction can be used in three ways, depending on the substance under 

Most of these procedures can be carried out on material cut to a particle size of less than 2 mm diameter - it is often advantageous to produce material of a smaller size and with a large surface area to mass ratio. This is conveniently done by grinding at the temperature of liquid nitrogen using an efficient and easily cleaned cutter mill. 

The extraction of additives strongly adsorbed or chemisorbed on the polymer - filler matrix must be carefully observed by the analyst, as a change of the method of manufacture of, for example, the filler or in the method of compounding the plastic formulation, can 

In a modification of this procedure the polymer is refluxed with a reagent, which decomposes additives present to put them in a form, which is soluble in the solvent. Thus when PP on which is chemisorbed fatty acid amides or amines, is refluxed with a solution of ethylene dichloride and trichloroacetic acid then the amides are decomposed as follows  

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Fractional extraction may sometimes find application, since the components distribute themselves in a different proportion in the solvent (compare Section 11,44). 

The physical process of Hquid—Hquid extraction separates a dissolved component from its solvent by transfer to a second solvent, immiscible with the first but having a higher affinity for the transferred component. The latter is sometimes called the consolute component. Liquid—Hquid extraction can purify a consolute component with respect to dissolved components which are not soluble in the second solvent, and often the extract solution contains a higher concentration of the consolute component than the initial solution. In the process of fractional extraction, two or more consolute components can be extracted and also separated if these have different distribution ratios between the two solvents. 

Liquid—Hquid equiHbria having more than three components caimot as a rule be represented on a two-dimensional diagram. Such systems are important in fractional extraction, for example, operations in which two consolute components C and D are separated by means of two solvents A and B. For the special case where A and B are immiscible, the linear distribution law can be appHed to components C and D independendy ... 

Dual solvent fractional extraction (Fig. 7b) makes use of the selectivity of two solvents (A and B) with respect to consolute components C and D, as defined in equation 7. The two solvents enter the extractor at opposite ends of the cascade and the two consolute components enter at some point within the cascade. Solvent recovery is usually an important feature of dual solvent fractional extraction and provision may also be made for reflux of part of the product streams containing C or D. Simplified graphical and analytical procedures for calculation of stages for dual solvent extraction are available (5) for the cases where is constant and the two solvents A and B are not significantly miscible. In general, the accurate calculation of stages is time-consuming (28) but a computer technique has been developed (56). 

Fractional extraction has been used in many processes for the purification and isolation of antibiotics from antibiotic complexes or isomers. A 2-propanol—chloroform mixture and an aqueous disodium phosphate buffet solution are the solvents (243). A reciprocating-plate column is employed for the extraction process (154). 

Liquid-liquid fractionation, or fractional extraction (Fig. 15-6), is a sophisticated scheme for nearly complete separation of one solute from a second solute by liquid-liquid extraclion. Two immiscible liquids travel countercurrently through a contaclor, with the solutes being fed near the center of the contactor. The ratio of immiscible-liquid flow rates is operated so that one of the phases preferentially moves the first solute to one end of the contactor and the other phase moves the second solute to the opposite end of the contactor. Another way to describe the operation is that a primaiy solvent S preferentially extracts, or strips, the first solute from the feed F and a wash solvent... 

In this work a novel five-step leaching scheme for HM has been developed addressing exchangeable, acid soluble (carbonate), easily reducible (bound to Mn oxides), easily oxidizable (bound to humic and fulvic acids), and moderately reducible (bound to amorphous Ee oxides) fractions extractable by 0.05 M Ca(N03), 0.43 M CH3COOH, 0.1 M NH,OH-HCl (non-acidified), 0.1 M K/,03 (pH 11), and 0.1 M (NH4),C,04 (pH 3), respectively. The sequence of extractants was chosen according to recent studies on the selectivity of leachants toward dissolved phases of soils. 

Fig. 5-11. Fractional extraction with gel-coated hollow fibers [57].

An unusual reaction is used to form a KRe 4 HjO. The reduction of potassium perrhenate in en-H20 solutions by potassium metal yields a white solid containing the Rh ion mixed with KOH. Extraction with isopropyl alcohol gives a colloidal brown liquid containing a mixture of KOH, isopropyl alcohol and the rhenidc. Fractional extraction of the liquid gives a gray solid that contains 5.5-60% KRe 4 HjO... 

The traditional use of SFE involved fractional extraction in which a selected group of oleoresin components is targeted. This technique makes it possible to extract subsequently the volatile oils (light fraction, under milder conditions, 120 bar, 40 C)... 

Fractional extraction occasionally is employed. The polymers of lowest molecular weight are extracted first from the sample, which is... 

These opposing tendencies may defeat the purpose of the fractional precipitation process. The fractional precipitation of crystalline polymers such as nitrocellulose, cellulose acetate, high-melting polyamides, and polyvinylidene chloride consequently is notoriously inefficient, unless conditions are so chosen as to avoid the separation of the polymer in semicrystalline form. Intermediate fractions removed in the course of fractional precipitation may even exceed in molecular weight those removed earlier. Separation by fractional extraction should be more appropriate for crystalline polymers inasmuch as both equilibrium solubility and rate of solution favor dissolution of the components of lowest molecular weight remaining in the sample. 

Fractional extraction Concentration in X-phase Concentration in Y-phase... 

Figure 5.191. Increasing both flow rates by a factor of 10 results in much lower fractional extraction values for these equilibrium stages.

Increased the sensitivity of this bloassay to 0.5 nM concentrations of allelochemlcals. The Lemna assays were also useful for determining bloactlve fractions extracted from allelopathic plants. 

Conventional methods of polymer extraction use large quantities of solvents as in shake-flask extraction or a Soxhlet extraction apparatus. For all classical extraction methods, solvent selectivity, in general, is low, i.e. solvents with high capacity tend to have low selectivity. In reflux extractions, which are still quite popular in polymer applications, the polymer is refluxed with a hot solvent, which disperses it to provide a solvent phase containing additives. In these conditions solvents are at their atmospheric boiling point. These methods are lengthy and labour intensive. Fractional extraction is based on solvents with increasing solvent power (cf. also [81]). 

Applications References [99-102] have reported fractional extraction of cresolic and phenolic antioxidants from PE. Conventional analysis of PVC compounds requires the subsequent use of various solvents... 

Many analytical techniques are in use for the qualitative and quantitative evaluation of monomers and oligomers extracted from PA6 (GC, differential refrac-tometry, IR, PC, SEC, HPLC, RPLC, etc.). FTIR has been used for quantitative analysis of caprolactam oligomer content (extract %) in polyamide-6 [113], The method, which involves a 3h extraction in boiling methanol, is suitable for process control and plant environment. Kolnaar [114] has used FTIR characterisation of fractional extracts with pentane, hexane, and heptane of HDPE for blow moulding applications. Vinyl acetate in packaging film has similarly been determined by quantitative FUR. 

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