Residual acidity

Di lve 20 g. of the cyano ester in 100 ml. of rectified spirit and add a solution of 19 2 g. of pure potassium cyanide in 40 ml. of water. Allow to stand for 48 hours, then distil oflF the alcohol on a water bath. Add a large excess of concentrated hydrochloric acid and heat under reflux for 3 hours. Dilute with water, saturate the solution with ammonium sulphate, and extract with four 75 ml. portions of ether. Dry the combined ethereal extracts with anhydrous sodium or magnesium sulphate, and distil off the ether. RecrystaUise the residual acid from excess concentrated hydrochloric acid, and dry in the air. The yield of pure ew-dimethyl-succinic acid, m.p. 141-142°, is 12 g. 

Cautiously add 250 g. (136 ml.) of concentrated sulphuric acid in a thin stream and with stirring to 400 ml. of water contained in a 1 litre bolt-head or three-necked flask, and then dissolve 150 g. of sodium nitrate in the diluted acid. Cool in a bath of ice or iced water. Melt 94 g. of phenol with 20 ml. of water, and add this from a separatory funnel to the stirred mixture in the flask at such a rate that the temperature does not rise above 20°. Continue the stirring for a further 2 hours after all the phenol has been added. Pour oflF the mother liquid from the resinous mixture of nitro compounds. Melt the residue with 500 ml. of water, shake and allow the contents of the flask to settle. Pour oflF the wash liquor and repeat the washing at least two or three times to ensure the complete removal of any residual acid. Steam distil the mixture (Fig. II, 40, 1 or Fig. II, 41, 1) until no more o-nitrophenol passes over if the latter tends to solidify in the condenser, turn oflF the cooling water temporarily. Collect the distillate in cold water, filter at the pump, and drain thoroughly. Dry upon filter paper in the air. The yield of o-nitrophenol, m.p. 46° (1), is 50 g. 

Strongly acidify the residual sodium bicarbonate solution to Congo red with dilute sulphuric acid. If a sohd acid forms, filter. Extract the filtrate or the acidified solution with two 20 ml. portions of ether keep the aqueous solution A). Distil off the ether, and add the residual acid (if a sohd) to the solid separated by filtration. Identify the acid. 

Methanol can be converted to a dye after oxidation to formaldehyde and subsequent reaction with chromatropic acid [148-25-4]. The dye formed can be deterruined photometrically. However, gc methods are more convenient. Ammonium formate [540-69-2] is converted thermally to formic acid and ammonia. The latter is trapped by formaldehyde, which makes it possible to titrate the residual acid by conventional methods. The water content can be determined by standard Kad Eischer titration. In order to determine iron, it has to be reduced to the iron(II) form and converted to its bipyridyl complex. This compound is red and can be determined photometrically. Contamination with iron and impurities with polymeric hydrocyanic acid are mainly responsible for the color number of the merchandized formamide (<20 APHA). Hydrocyanic acid is detected by converting it to a blue dye that is analyzed and deterruined photometrically. 

As Eigure 1 implies, there is usually some residual acidity as well as free hydroxyl groups left in the resin molecules. Stmcture-property relationships and the principles commonly followed to design the resin stmcture are discussed later. 

The ratio of cycHc to linear oligomers, as well as the chain length of the linear sdoxanes, is controlled by the conditions of hydrolysis, such as the ratio of chlorosilane to water, temperature, contact time, and solvents (60,61). Commercially, hydrolysis of dim ethyl dichi oro sil a n e is performed by either batch or a continuous process (62). In the typical industrial operation, the dimethyl dichi orosilane is mixed with 22% a2eotropic aqueous hydrochloric acid in a continuous reactor. The mixture of hydrolysate and 32% concentrated acid is separated in a decanter. After separation, the anhydrous hydrogen chloride is converted to methyl chloride, which is then reused in the direct process. The hydrolysate is washed for removal of residual acid, neutralized, dried, and filtered (63). The typical yield of cycHc oligomers is between 35 and 50%. The mixture of cycHc oligomers consists mainly of tetramer and pentamer. Only a small amount of cycHc trimer is formed. 

Such a reaction is controlled by the rate of addition of the acid. The two-phase system is stirred throughout the reaction the heavy product layer is separated and washed thoroughly with water and alkaU before distillation (Fig. 3). The alkaU treatment is particularly important and serves not just to remove residual acidity but, more importantiy, to remove chemically any addition compounds that may have formed. The washwater must be maintained alkaline during this procedure. With the introduction of more than one bromine atom, this alkaU wash becomes more critical as there is a greater tendency for addition by-products to form in such reactions. Distillation of material containing residual addition compounds is ha2ardous, because traces of acid become self-catalytic, causing decomposition of the stiU contents and much acid gas evolution. Bromination of alkylthiophenes follows a similar pattern. 

Schollenberger added 2% of a polycarbodiimide additive to the same poly(tetra-methylene adipate) urethane with the high level of acid (AN = 3.66). After 9 weeks of 70°C water immersion, the urethane was reported to retain 84% of its original strength. Carbodiimides react quickly with residual acid to form an acyl urea, removing the acid catalysis contributing to the hydrolysis. New carbodiimides have been developed to prevent hydrolysis of polyester thermoplastics. Carbodiimides are also reported to react with residual water, which may contribute to hydrolysis when the urethane is exposed to high temperatures in an extruder [90]. 

Chemical Reactivity - Reactivity with Water Dissolves and reacts to form acid solution and toxic red oxides of nitrogen Reactivity with Common Materials Corrosive to most metals, but reaction is not hazardous Stability During Transport Stable Neutralizing Agents for Acids and Caustics Flush with water. Residual acid may be neutralized with soda ash Polymerization Not pertinent Inhibitor of... 

The resin bed is brought in con- tact with the regenerant solution. In the case of the cation resin, acid elutes the collected ions and converts the bed to the hydrogen form. A slow water rinse then removes any residual acid. 

Protein-Pak packings are designed for the size exclusion chromatography of proteins and related compounds. They are based on silica, which is deactivated with glycidylpropylsilane. The diol function prevents the interaction of the target analytes with the silica surface. However, because coverage of the silica surface is always incomplete, residual acidic silanols can interact with the analytes. For this reason, most applications are carried out with a salt concentration above 0.2 mol/liter, which eliminates the interaction of analytes with surface silanols. Protein-Pak packings are stable from pH 2 to pH 8. 

Other workers have obtained higher yields of phenylethanol is absolute methanol the 90% yield reported above was probably due to traces of residual acid remaining from the catalyst preparation. Note that hydrogenolysis with this catalyst can be prevented completely by traces of base addition of base is often a useful means of preventing or minimizing unwanted hydrogenolysis in a variety of systems. 

Unrecognized traces of residual acids or bases in catalysts is one reason investigators have failed to duplicate the work of others (or their own). On the other hand, this variable often has little or no influence. Acidity of a catalyst can be readily checked by slurring it in water and measuring the pH. 

The products of the solvent extraction process are tantalum strip solution, niobium strip solution and raffinate - liquid wastes containing impurities and residual acids. 

The first purification step is thorough washing of the TNT with hot water, in washing tanks or by emulsification, followed by neutralization with Na bicarbonate soln. This removes residual acids... 

A significant improvement in yield (to about 74%) and purity (approx 98%) was realized by the substitution of methanol for chlf and crystn of the product from the soln without neutralization, residual acid being removed, by washing the filter cake with w... 

Polyester polyols (Scheme 4.4) are prepared by condensation polymerization of dicarboxylic acids and diols. An excess of diol ensures OH functional product, minimizing die possibility of residual acid groups which react with isocyanates to generate C02 and act as inhibitors in catalyzed urethane reactions. The reactants are heated at 200-230°C under vacuum to remove the water by-product and drive the reaction to completion. The most common coreactants include adipic... 

When the iron-based catalyst 66 was used, a high level of enantiomeric excess in the cycloadditions between cyclopentadiene (18) and a,/i-unsaturated aldehydes [65] was observed. The cycloadditions were carried out in the presence of 2,6-di-t-butylpyridine (Scheme 3.15) which was added to scavenge residual acid impurities. 

Extraction procedures must be adjusted when separated anthocyanins will be tested in biological studies. We have found that the types of acids used for anthocyanin extraction as well as their residual concentrations in the final extract may affect the results obtained from biological tests. The growth inhibitory effect of anthocyanins on HT29 (human colonic cancer) cells may be overestimated if the residual acid in the extract exerts a toxic effect on the cells. Acetic acid residues in anthocyanin extracts showed less toxicity to HT29 cells than hydrochloric acid when samples were prepared under the same extraction procedure and subjected to the same tests on HT29 cells. In addition, the procedure to remove acids affected the acid residual concentration as well in final anthocyanin extracts, with lyophilization being more successful than rotary evaporation. 

After the addition of acid chloride, about 25 ml of methylene chloride was used to rinse the residual acid chloride into the flask. The mixture was stirred for about 3 h. The pH was then adjusted to between 9.5 and 10 and the solution was stirred for an additional hour. The organic layer was separated from the aqueous layer and washed once with 5% NaOH solution. The solution was dried over calcium sulfate and the methylene chloride was evaporated leaving about 10.36 g (69%) of crude product. Decolorizing three times with Attapulgus clay yielded a light yellow brown methylene chloride solution which, on removal of solvent, gave about 5.2 g of product (35%). 

Spent pickle liquor in the acid pickling wastewaters is listed as hazardous waste K062, regulated under RCRA, as it contains considerable residual acidity and high concentrations of dissolved iron salts.2 Exhausted pickling baths are mainly composed of nitrate (150 to 180 g/L), fluoride (60 to 80 g/L), iron (III) (30 to 45 g/L), chromium (III) (5 to 10 g/L), and nickel (II) (3 to 5 g/L). 

Spent pickle liquor is considered a hazardous waste (K062) because it contains considerable residual acidity and high concentrations of dissolved iron salts. For example, spent pickle liquor and waste acid from the production of stainless steel is considered hazardous. The hazardous constituents in K062 are lead, nickel, and hexavalent chromium. Waste pickle liquor sludge generated by lime stabilization of spent pickle liquor is not considered hazardous unless it exhibits one or more of the characteristics of hazardous waste. An estimated 6 million tons of spent pickle liquor are generated annually in the U.S.1... 

Pd is the most widely used catalyst for the cleavage of benzylic C—O bonds, and 10% Pd/C is the most popular form of Pd for hydrogenolysis of benzyl alcohols. This catalyst usually contains residual acids, which increase reaction rates. 

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