Extractives appropriate solvents

In the manufacture of base oils, one of the refining operations is to extract with the aid of an appropriate solvent (furfural most often) the most aromatic fractions and the polar components. When free of solvent, the extracted aromatic fraction can eventually be refined, particularly to remove color or to thicken it, or still further, to fractionate it. The term, aromatic extract is used in every case. 

Endo-exo product mixtures were isolated using the following procedure. A solution of cyclopentadiene (concentration 2-10" M in water and 0.4 M in oiganic solvents) and the dienophile (concentration 1-5 mM) in the appropriate solvent, eventually containing a 0.01 M concentration of catalyst, was stirred at 25 C until the UV-absorption of the dienophile had disappeared. The reaction mixture (diluted with water in the case of the organic solvents) was extracted with ether. The ether layer was washed with water and dried over sodium sulfate. After the evaporation of the ether the... 

In the wood rosin process, rosin is isolated from aged pine stumps that have been left in fields cleared for farming or lumbering operations. The stumps are cut and shredded to pieces the size of matchsticks. The wood chips are then extracted with an appropriate solvent, eg, aUphatic or aromatic petroleum hydrocarbons or ketones. The extract is fractionally separated into nonvolatile cmde rosin, volatile extractibles, and recovered solvent. The dark rosin is usually refined further to lighter-colored products using selective solvents or absorption. 

A critical study has been carried out in order to evaluate the capabilities of Near Infrared spectroscopy for the analysis of commercial pesticide formulations using transmittance measurements. In this sense, it has been evaluated the determination of active ingredients in agrochemical formulations after extraction with an appropriate solvent. 

Theoretical and applied aspects of microwave heating, as well as the advantages of its application are discussed for the individual analytical processes and also for the sample preparation procedures. Special attention is paid to the various preconcentration techniques, in part, sorption and extraction. Improvement of microwave-assisted solution preconcentration is shown on the example of separation of noble metals from matrix components by complexing sorbents. Advantages of microwave-assisted extraction and principles of choice of appropriate solvent are considered for the extraction of organic contaminants from solutions and solid samples by alcohols and room-temperature ionic liquids (RTILs). 

To the epoxide dissolved in a minimal amount of chloroform or ether is added a corresponding solution of freshly prepared thiocyanic acid (20 fold excess) as described above (acetic acid has also been used as solvent). The resulting solution is allowed to stand at least 70 hr at room temperature. (Some workers have protected the reaction mixture from light during this period). The reaction mixture is worked up by washing first with a 10% solution of sodium carbonate, sodium bicarbonate or potassium bicarbonate, and then water. The remaining ether extract is dried (Na2S04) and evaporated under vacuum. The crude thiocyanatohydrin is crystallized from an appropriate solvent or treated with methanesulfonyl chloride s (see below). 

A solution of the acylated thiocyanatohydrin in a minimal amount of 5% potassium hydroxide in diglyme (other solvents such as methanol, ethanol or tetrahydrofuran have also been used) is stirred for 2 days at room temperature. Water is added to the reaction mixture to precipitate the product which is filtered or extracted with ether (or chloroform). The ether extract is washed several times with water, dried (Na2S04), and concentrated under vacuum. The thiirane usually can be crystallized from an appropriate solvent pair. Chromatography over alumina has been used for the purification of episulfides. 

The direct mode is used when the concentration of the SEE extract is enough for direct analysis in the CE instrument without the need for a pre-concentration step. In this case, the sample concentrator is by-passed and the SEE extract goes directly to the CE instrument. The extract is collected in a CE vial containing an appropriate solvent and is thus ready for the CE analysis (Eigure 6.12). 

Equiv of the imine 2 is dissolved in the appropriate solvent and 1 cquiv of the silyl ketene acetal 1 is added, the mixture is cooled to —70 °C and 0.1 equiv of TMSTf is added. After 15 h the reaction is quenched with H.O. 10% aq NH40H is added to make the piT basic, and the reaction mixture is extracted with F.tOAc. The crude product (obtained after the usual workup) is subjected to silica gel chromatography (pet. cthcr/Et20) to give the pure /J-amino ester 3. 

This sample preparation required both extraction and concentration and this was carried out in the traditional manner with the use of an appropriate solvent. The separation was again achieved exploiting the dispersive interactions between the components of the mixture and the strongly dispersive hydrocarbon chains on the reversed phase. 

Entrapment of enzymes within reversed micelles can be achieved simply by dissolving the biopolymer, pure or solubilized in an appropriate solvent, in a solution of reversed micelles or by extraction from an immiscible liquid phase [13,165,166]. 

A sequential analysis protocol includes three steps (1) extraction in water or other appropriate solvent for the colorant, (2) purification or concentration of the colorant, and (3) separation coupled with detection of the target molecule. Different methods of extracting synthetic colorants from foods have been developed using organic solvents followed by SPE protocols using as adsorption support RP-C18, amino materials, or Amberlite XAD-2. Eor qualitative evaluations, the easiest option for separating colorant molecules from unwanted ingredients found in an extract is SPE on polyamide or wool. 

Improved Methods for Collection, Bioassay, Isolation, and Characterization of Compounds. Techniques used to characterize natural products are evolving rapidly as more sophisticated instrumentation is developed. Plant physiologists and chemists should work closely together on this aspect, since rapid and reproducable bioassays are essential at each step. There is no standard technique that will work effectively for every compound. Briefly, isolation of a compound involves extraction or collection in a appropriate solvent or adsorbant. Commonly used extraction solvents for plants are water or aqueous methanol in which either dried or live plant parts are soaked. After extracting the material for varying lengths of time, the exuded material is filtered or centrifuged before bioassay. Soil extraction is more difficult, since certain solvents (e.g. bases) may produce artifacts. 

Principles and Characteristics A first step in additive analysis is the identification of the matrix. In this respect the objective for most polymer analyses for R D purposes is merely the definition of the most appropriate extraction conditions (solvent choice), whereas in rubber or coatings analysis usually the simultaneous characterisation of the polymeric components and the additives is at stake. In fact, one of the most basic tests to carry out on a rubber sample is to determine the base polymer. Figure 2.1 shows the broad variety of additive containing polymeric matrices. 

When using any solvent extraction system, one of the most important decisions is the selection of the solvent to be used. The properties which should be considered when choosing the appropriate solvent are selectivity distribution coefficients insolubility recoverability density interfacial tension chemical reactivity viscosity vapour pressure freezing point safety and cost. A balance must be obtained between the efficiency of extraction (the yield), the stability of the additive under the extraction conditions, the (instrumental and analyst) time required and cost of the equipment. Once extracted the functionality is lost and... 

Applications Extraction is typically accomplished by refluxing the polymer in an appropriate solvent for l-48h [84,199]. In many cases, ultrasonic exposure reduces the extraction time [90,200], According to Table 3.5 there are several reports of US extraction from polymers. Ultrasonic extraction has been used for HDPE/(BHT, Irganox antioxidants, Isonox, Cyasorb, Am 340, MD 1024, Irgafos 168) [56], LDPE/Chimassorb 81 [201], SBR/tri(nonylphenyl) phosphite [200], HDPE/(Tinuvin 770, Chimassorb 944) [114], etc. Nielson [90] compared the recoveries obtained for a variety of analytes from PP, LDPE and HDPE with Soxhlet, ultrasonic bath and microwave oven. For all samples, the ultrasonic extraction could be achieved within 1 h. For LDPE and PP most compounds (except Irganox 1010) were extracted within 10 min. Further experiments by Nielson [56] on extraction from HDPE confirmed these results. Where phosphite antioxidants (such as Irgafos 168) are present the use of the solvent mixture DCM-cyclohexane was preferred as it prevented hydrolysis of the phosphite by extraction solvents such as alcohols [56]. Similarly, phosphite esters also undergo hydrolysis... 

Several authors [92,292,317] have discussed a number of factors affecting SFE from polymers. All classic and new extraction techniques require pre-extraction procedures to ensure that appropriate solvent contact is maximised for solid and semisolid matrices. The preextraction strategies for SFE are given in Table 3.17. 

Specification of acceptable limits on extractables is preferred when possible by regulatory authorities. At a minimum, a profiling of extractables using appropriate solvents is expected of pharmaceutical manufacturers. 

An alternative to the extraction of intact PHA polymer is the isolation of PHA monomers, oligomers, or various derivatives such as esters [74]. PH As are composed of stereo-chemically pure P-3-hydroxyacids, and therefore can be used as a source of optically pure organic substrates for the chemical and pharmaceutical industry [79]. In this protocol, the defatted cake containing PHA polymer would be chemically treated to obtain the PHA derivatives. For example, transesterification of the meal with methanol would give rise to methyl esters of 3-hydroxyalkanoic acids. The PHA derivatives would then be separated from the meal with appropriate solvents. One potential disadvantage of this method is the potential alteration of the quality of the residual meal if the harsh chemical treatments required for the production of PHA derivatives lead to protein or amino acid breakdown. 

Consider the analysis of plant material for a pesticide residue by GC. Two grams of the material is chopped up and placed in a Soxhlet extractor (Chapter 11) and the pesticide quantitatively extracted into an appropriate solvent. Following this, the solvent is evaporated to near dryness and the residue is diluted to volume in a 25-mL flask. Then 2.5 pL of this solution and standards is injected in a GC with the following results ... 

The extraction apparatus is used chiefly for dissolving out sparingly soluble constituents from mixtures, and for isolating natural products from (dry) vegetable or animal material. Occasionally it is very useful for recrystallising sparingly soluble substances from the extraction thimble by means of an appropriate solvent (especially ether). As a rule, crystals of the dissolved material separate already from the solution in the flask during the process of extraction. This solution soon becomes supersaturated even while hot. 

The oil has to be removed from the SSP product by extraction or flushing with appropriate solvents such as acetone. The degree of swelling influences abrasion and the loss of fines, as well as a certain tendency to a form of sticking or adhesion. At present, this method does not appear to have been fully commercialized. 

Following dialysis and treatment by SEC, the sample extracts were solvent exchanged into sterile DMSO. Subsequently, four rainbow trout Oncorhynchus mykiss [RBT]) were placed in each of seven tanks (each tank is considered as a treatment and a replicate is an individual fish within a tank) in 18 °C well water (280 mg hardness as CaCOs) using flow-through conditions. RBT were fed once daily throughout the study. Following a 48 hour acclimation, RBT were injected interperitoneally with 100 pL of a 1 1 mixture of an SPMD extract or appropriate controls in DMSO or corn oil. Controls included non-deployed SPMD extracts, SEC blanks, and DMSO blanks. The same injection procedure was repeated 6 days later. RBT were sacrificed 11 days after initial exposure to the extracts, and the plasma, liver, gills, and brain were immediately removed from each fish and maintained at -80 °C until assayed. 

Similarly, leaching of the wood in water after an appropriate solvent extraction does not prove that a chemical bond exists between the modificant and the wood. 

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