Insoluble fractions, separation

To produce highly purified phosphatidylcholine there are two industrial processes batch and continuous. In the batch process for producing phosphatidylcholine fractions with 70—96% PC (Pig. 4) (14,15) deoiled lecithin is blended at 30°C with 30 wt % ethanol, 90 vol %, eventually in the presence of a solubiHzer (for example, mono-, di-, or triglycerides). The ethanol-insoluble fraction is separated and dried. The ethanol-soluble fraction is mixed with aluminum oxide 1 1 and stirred for approximately one hour. After separation, the phosphatidylcholine fraction is concentrated, dried, and packed. 

In the continuous process for producing phosphatidylcholine fractions with 70—96% PC at a capacity of 600 t/yr (Pig. 5) (16), lecithin is continuously extracted with ethanol at 80°C. After separation the ethanol-insoluble fraction is separated. The ethanol-soluble fraction mns into a chromatography column and is eluted with ethanol at 100°C. The phosphatidylcholine solution is concentrated and dried. The pure phosphatidylcholine is separated as dry sticky material. This material can be granulated (17). 

The starting material is moderately soluble in hot chloroform, while 2-hydroxyisophthalic acid is quite insoluble. Fractional crystallization from water, an alternative method suggested for the separation of starting material, has been found by the submitters to be unsuccessful. 

Alcohol was then distilled off, until the temperature reached 100°C. 1,706.6 g of distillate was collected. (Theory 1,430 g.) This alcohol was poured into four times its volume of water and an insoluble oil separated (457 g). The insoluble fraction was added back to the copoly-... 

Speciation of plutonium leached from the glass cubes is shown in Figure 1. The first bar represents the total amount of insoluble plutonium and is the summation of suspended plutonium (the difference between the values for filtered and unfiltered waters) and sorbed plutonium—viz., the amount removed from the cubes by a 0.1 M perchloric acid wash, normalized to the volumes of leachant solutions so that it is comparable to the other values in the graphs. For simplicity, the insoluble fractions are combined in one bar, whereas the various oxidation states in the soluble fraction are represented by separate bars. It should be noted that the ordinate scale varies among the graphs. 

The HMR/fractionatlon approach gives very good results When applied to ethylene-propylene copolymer fractions reported by Abls, et. al. (19) These authors extracted sample 5 (In Table VII) with hexane to get soluble and Insoluble fractions (5a and 5b), and with ether to get soluble and insoluble fractions (5c and 5d). The hexane set (5a and 5b) and the ether set (5c and 5d) can be separately analyzed by the HIXCO.TRIADX program. The results are shown In Table VIII. In the 2-state (B/B) model, we have 4 parameters and 12 values to fit to HMR data of pairwise fractions. In the 3-state (B/B/B) model, we have 7 parameters and 12 values to fit. Thus, the use of pairwise fractions Is absolutely essential for 3-state analysis. 

CYCLOHEXANE EXTRACTION. A 5-6g portion of the product was cut into small pieces and stirred in 250 ml cyclohexane at room temperature for 60 hr. The insoluble fraction was separated by filtering the solution through cheesecloth. The cyclohexane-soluble fraction was recovered by distilling the solvent in vacuo and the polymer was dried in vacuo at 40 C for 24 hr. 

A similar procedure was described by Eboatu and Ferguson. An object of analysis was the complex obtained by template polymerization of acrylic acid in the presence of poly(vinyl pyrrolidone). The polycomplex was dispersed in dry benzene and treated with diazomethane. The insoluble portion was filtered. The filtrate containing poly(methyl acrylate) was concentrated and finally dried. The insoluble fraction was scrubbed with methanol to extract polyCvinyl pyrrolidone). The residue was further washed with methanol and then dried. These three portions were characterized by IR spectroscopy. It was found that only about 70% separation of the complex is achieved. The occurrence of inseparable portion is attributed to a graft copolymer formation. For the separated... 

Contrary to the copolymerization in THF, the copolymer zation in toluene proceeded abnormally, i.e. it formed an isotactic homopolymer of MMA and a copolymer with low stereoregularity. The copolymerization of an equimolar mixture of MMA and TrMA was carried out in toluene with BuLi at -78°C, and the polymer obtained was treated in methanolic hydrochloric acid in order to hydrolyze selectively the TrMA units into methacrylic acid units. Then the resulting polymer was separated into two fractions with methanol, as shown in Table . The methanol insoluble fraction was found... 

Figure 15. UV spectra of Fraction 1, 2, and 3 separated from the aminopropanol extract of the water and salt-solution insoluble fraction of LCP cottonseed flour (4)...

In contrast. Figure 2 shows that the percentage of protein in solution for soy isolates remains constant as the amount of added protein is increased (1 ). In other words, the amount of protein in solution increases linearly with increasing amounts of added protein. This behavior is observed for all the isolates we have studied up to the highest concentration of 18 percent. Thus, soy isolates behave as if they are composed of a completely soluble fraction (A) and a completely insoluble fraction (B). Upon the addition of solvent, the soluble fraction (A) dissolves completely while the insoluble fraction (B) remains unchanged. There is no equilibrium established between A and B such that, if B is separated from A and reslurried in additional amounts of solvent, no additional protein will go into solution. (More precisely, no evidence of microscopic reversibility was found on the time scale of the experiment,... 

The extract yields are shown in Table II. More than 90% of the organic coal substance was dissolved in the extraction of Ireland Mine vitrain concentrate and about 85% in the case of Bruceton coal. The yield of the phenanthrene soluble fraction was not determined in the extraction of Ireland Mine coal. In that run the products were worked up with a different procedure, and the phenanthrene soluble and phenanthrene insoluble fractions were not separated. 

Heidelberger and Aisenberg240 studied the cross-reaction of the Merck and DuPont polyglucoses with antibodies to pneumococcal C-substance and to type-specific polysaccharides. One of the D-glucose polymers (Merck 52R61I) was separated into a series of fractions on the basis of fractionation with alcohol (isopropyl alcohol and ethanol) and with glacial acetic acid, the most insoluble fraction being called A, and the most soluble, E. The yield, analyses, and reactivity of these fractions with Types IX, XII, XX, and XXII antipneumococcal horse sera are presented in Table VII. 

Invertase from a Saccharomyces cerevisiae mutant could be separated into two fractions on the basis of solubility in ammonium sulfate.382 The soluble fraction reacted with endo-(l - 6)-a-mannanase, when it became insoluble. The results suggested that the insoluble fraction contained only the highly branched, core section, but the soluble fraction also had the (l->6)-a-D-mannan chain attached. 

The soluble and insoluble fractions were examined separately. The insoluble fraction, which made up 35% of the total, had the NMR spectrum expected of a DPP-rich block copolymer, with a sharp methyl proton signal and only one strong signal, at 8 6.46 ppm (PPP), in the aromatic backbone region. The composition, from comparison of the integrated intensities of the methyl and backbone proton signals, was 82 mole % DPP and 18% MPP. The soluble fraction had the spectrum expected of a block copolymer with about 65% MPP units. Since a coprecipitated blend was separated almost quantitatively into the pure homopolymers with m-xylene under these conditions, the copolymer is characterized as a block copolymer. 

In water studies it is standard practice to filter the sample soon after collection, usually through a 0.45p,m membrane disc (made of cellulose acetate, cellulose nitrate or polycarbonate). This process arbitrarily divides the sample components into soluble and insoluble fractions, but as shown in Table 2.3, the average size of different chemical species varies widely, and some differentiation between species can be obtained through using filter media of different pore sizes. For example, fully dissolved compounds can be separated from finer colloidal forms by using gel filtration and dialysis, and sub-division of the total content into fractions based on particle or molecular size (see Section 2.3) has been used for speciation of elements in waters. 

An operational definition is considerably more practical. Operationally determined species are defined by the methods used to separate them from other forms of the same element that may be present. The physical or chemical procedure that isolates the particular set of metal species is used to define the set. Metals extracted from soil with an acetate buffer is an operational definition of a certain class. Lead present in airborne particles of less than 10 pm is another. In water analyses, simply filtering the sample before acidification can speciate the analytes into dissolved and insoluble fractions. These procedures are sometimes referred to as fractionation, which is probably a more properly descriptive term than speciation, as speciation might imply that a particular chemical species or compound is being determined. When such operational speciation is done, careful documentation of the protocol is required, since small changes in procedure can lead to substantial changes in the results. Standardized methods are recommended, as results cannot be compared from one laboratory to another unless a standard protocol is followed [124], Improvements in methodology must be documented and compared with the currently used standard methods to produce useful, readily interpretable information. 

A colorimetric method has been used by Meyer 9 to determine the size of fractions of degraded liver glycogen. A glycogen having a molecular weight of 290,000 was separated by electrodecantation into a soluble fraction whose value was 95,000, and an insoluble fraction whose value was 320,000. 

Figure 1 represents a schematic illustration of the separation of ribosomes, sRNA, and the enzymes involved in the transfer reaction, described in detail below. At the end of the incubation period, the ribonucleoprotein and supernatant fractions were separated by ultracentrifugation, the perchloric acid-insoluble fraction was prepared from each, and the nucleic acids and proteins were isolated from the acid-insoluble residue (17). 

In studies running parallel to carbonization with catalysts, Mochida et al. (78, 81) studied the separation of parent feedstocks into benzene-soluble (BS) and benzene-insoluble fractions(BI) and attempted co-carbonization of blends of these fractions. In addition, certain fractions were hydrogenated or alkylated and these alkylated fractions themselves hydrogenated. Mochida et al. (78-81) were looking for Compatibility between fractions, that is the ability of a blend of fractions to carbonize to a needle-coke. The commercial application of good compatibility could involve the use of low percentage additions of an active fraction (component) to produce a good needle-coke. 

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