Phenolics-neutrals fraction

In a polyphenolic extract, anthocyanins can interfere with other polyphenolics such as pro-cyanidins during HPLC analysis and hence should be removed prior to analysis. Anthocyanins from crude polyphenolic extracts can be removed as described in Basic Protocol 2. The ethyl acetate used for elution of phenolic compounds other than anthocyanins is removed using a rotary evaporator at 20°C. The non-anthocyanin polyphenolics are dissolved in deionized distilled water and the pH is adjusted to 7.0 with NaOH as described in Alternate Protocol 2 or the method developed by Oszmianski and Lee (1990a). In the latter method, polyphenolics were fractionated into three groups neutral fraction A (flavanols and other polar phenolics), neutral fraction B (flavonols), and acidic phenolics. Polyphenolic extracts were adjusted to pH 7.0 with NaOH... 

Because phenols are weak acids, they can be freed from neutral impurities by dissolution in aqueous N sodium hydroxide and extraction with a solvent such as diethyl ether, or by steam distillation to remove the non-acidic material. The phenol is recovered by acidification of the aqueous phase with 2N sulfuric acid, and either extracted with ether or steam distilled. In the second case the phenol is extracted from the steam distillate after saturating it with sodium chloride (salting out). A solvent is necessary when large quantities of liquid phenols are purified. The phenol is fractionated by distillation under reduced pressure, preferably in an atmosphere of nitrogen to minimise oxidation. Solid phenols can be crystallised from toluene, petroleum ether or a mixture of these solvents, and can be sublimed under vacuum. Purification can also be effected by fractional crystallisation or zone refining. For further purification of phenols via their acetyl or benzoyl derivatives (vide supra). 

Isolation of Antimicrobial Alkaloids from Tertiary Non-phenolic Base Fraction - A 2 g portion of the crude nonphenolic base fraction was dissolved in chloroform and chromatographed over 200 g of aluminum oxide (Woelm, neutral, grade III). The solvents used were 300 ml of chloroform, 500 ml of 1Z methanol in chloroform, 300 ml of 2Z metha-... 

Eor obtaining neutral fraction the column was eluted with water firstly. The acidic fractions were obtained by elution of linear NaCI gradient (0-1.4 M) in water. The carbohydrate elution profile was determined using the phenol-sulphiric acid method, finally two column volumes of a 2 M sodium chloride solution in water were eluted to obtain the most acidic polysaccharide fraction. The relevant fractions based on the carbohydrate profile were collected, dialysed and lyophilized. 

We found that the ether and ethyl acetate extracts of chicory roots exhibited the best nematicidal activities. The extracts were separated according to their acidity to give organo-acidic, phenolic, basic and neutral fractions. The phenolic fraction was found... 

When worked up sequentially with sodium bisulfite, sodium bicarbonate, and sodium hydroxide, the noncarbohydrate portion divides into fractions rich in aldehyde groups, carboxyl groups, and free phenolic hydroxyl groups, all exhibiting strong aromatic bands in infrared spectra (Figure 5). A fourth fraction remains after extraction by the other three reagents which shows some hydroxyl and aldehydic functionality but mainly aliphatic hydrocarbon structure. This neutral fraction is derived... 

Total Carboxyl and Phenolic Hydroxyl Content Conductimetric titrations employed were modifications of the procedure described by Sarkanen and Schuerch (11) for lignin total phenolic content. Spectroscopic determinations on the phenolics and neutrals fractions were carried out using the JEOL FX-900 Fourier Transform NMR spectrometer and the Nicolet 5SXC Fourier Transform Infrared Spectrometer. In addition, the solid state CP/MAS 13C-NMR spectra were obtained by the Regional NMR Center at Colorado State University using conditions described in Bryson et al. (12). 

Figure 6. CP/MAS 13C-NMR of novolaks a) phenol-formaldehyde b) phe-nol phenols/neutrals (1 1) pine sawdust pyrolysis oil fraction and formaldehyde.

Figure 7. Amortized costs of phenolics and neutrals fraction from pine sawdust pyrolysis calculated as a function of feedstock cost and plant size. Note that the calculations include costs associated with all feedstock preparation as if this were an independent plant.

Neutralized cleavage effluent is first split into separate acetone/ cumene/AMS/water and phenol/heavier fractions (5). Overheads from the splitter are then fractionated to remove aldehydes (6) and cumene/ AMS/water (7) to produce high-purity acetone (99.75+ wt%). Splitter bottoms is fractionated undervacuum to producea crude phenol distillate (8) and a heavy waste hydrocarbon stream. Hydrocarbon impurities are removed from the crude phenol by hydroextractive distillation (9) followed by catalytic phenol treatment (10) and vacuum distillation (11) to produce ultra-high-purity phenol (+99.99 wt%). 

In Chapter 6 the use of isoprene (Table 6.1) and of geranyl halides in reactions with naphthol and phenol respectively has been briefly referred to. In early work, isoprene with phenol in toluene containing 71% phosphoric acid, when reacted over 16 hours at ambient temperature (ref. 2) gave 4-(3-methylbut-2-enyl)phenol, the corresponding 2- isomer and 4-(3-methyl-3-hydroxybutyl)phenol in the phenolic products and in the neutral fraction, smaller proportions of 2,2-dimethylchroman and 6-(3-hydroxyisopentyl)-2,2-dimethylchroman. Hydrogenation of the unsaturated phenols afforded the respective 4- and 2-isopentylphenols. 

The method is directed towards the particulates produced and excludes the volatile compounds of very low molecular weight. Smoke particulates from the smouldering of PU foam in air were collected on glass fibre filters and extracted with chloroform. The concentrated extract was subjected to acid and base extractions. The acid compounds were converted to methyl esters and analysed by a GC-MS data system. The basic and phenolic compounds were analysed using the same system without derivatisation. The neutral fractions were separated into different classes by high-performance liquid chromatography on a bonded amine column. Different fractions were collected and each fraction was analysed by GC-MS with data collection. 

We suspect that both neutral EDTA and water-autoclave extraction procedures readily recovered the free phenolic acid fraction. So how effective were they in extracting reversibly sorbed phenolic acids (i.e., sorbed recovered by neutral EDTA or water-autoclave extraction minus free recovered by water extraction) For the 1,000 p.g/g added 723 p.g/g was sorbed by Cecil A and 833 p,g/g by Cecil B. For Cecil A samples, 13% (96 of 723 tig/g) and 6% (45 of 723 p-g/g) of the sorbed ferulic acid was recovered by the neutral EDTA and the water-autoclave procedures, respectively. Of this 96% (92 pg/g) and 55% (25 pg/g), respectively, was utilized by microorganisms over the 30 days (Blum et al. 1992). For Cecil B samples, 43% (357 of 833 pg/g) and 16% (137 of 833 pg/g) of the sorbed ferulic acid was recovered by the neutral EDTA and the water-autoclave procedures, respectively. Of this 100% (357 pg/g) and 97% (133 pg/g), respectively, was utilized by microorganisms over the 30 days. 

The crude extracts contain, in addition to the ketosteroids, nonketonic, acidic, and phenolic material (estri ns) as well as pigments. The acidic material may be removed by washing with saturated sodium bicarbonate solution, the phenols by washing with normal sodium hydroxide solution, and the amount of pigment present in the extract may be reduced by washing with alkaline sodium dithionite solution. After removal of these undesired constituents of the crude extract, the ether or other organic solvent is distilled off, leaving behind the neutral fraction as residue. 

The neutral or unsaponifiable materials present in tall oil include anhydrides, phenolics, diterpene aldehydes and alcohols, stilbenes, and steroids. In the neutral fraction of southern pine tall oil soap, 80 compounds have been identified. They include 25.1 percent sistosterol and a total of 32.4 percent steroids. The sistosterol content of crude tall oil is 2 to 3 percent and is the main component of the neutral fraction. 

A mixture of monolauryl phosphate sodium salt and triethylamine in H20 was treated with glycidol at 80°C for 8 h to give 98% lauryl 2,3-dihydro-xypropyl phosphate sodium salt [304]. Dyeing aids for polyester fibers exist of triethanolamine salts of ethoxylated phenol-styrene adduct phosphate esters [294], Fatty ethanolamide phosphate surfactant are obtained from the reaction of fatty alcohols and fatty ethanolamides with phosphorus pentoxide and neutralization of the product [295]. A double bond in the alkyl group of phosphoric acid esters alter the properties of the molecule. Diethylethanolamine salt of oleyl phosphate is effectively used as a dispersant for antimony oxide in a mixture of xylene-type solvent and water. The composition is useful as an additive for preventing functional deterioration of fluid catalytic cracking catalysts for heavy petroleum fractions. When it was allowed to stand at room temperature for 1 month it shows almost no precipitation [241]. 

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