Ethanol VOLUME

Prepare four to six standard solutions of ethanol in water such that the alcohol content of the wine (as indicated on the wine label) is in the middle. For example, if the wine is 15% ethanol (volume percent assumed), standards of 5,10,20, and 25% are appropriate. Use 25-mL volumetric flasks, and pipet the ethanol accurately. Dilute to the mark with water and then add 1.00 mL of acetone (the internal standard) above the mark. Shake well. 

The progress of the partial saponification can be checked by a simple solubility test. About 1 ml of the solution is withdrawn and the cellulose acetate precipitated with water. The small sample is quickly washed free of acid and dried as much as possible by pressing between two filter papers. Some fibers of the still damp material are placed in a test tube with 15-20 ml oholuene/ethanol (volume ratio 1 1) and heated to boiling in a water bath. If the fibers go into solution, then after about 15 min the whole charge can be worked up as described above. 

Preliminary data on the reactivity of these materials in a typical Knoevenagel reaction (cyclohexanone and ethyl cyanoacetate) indicates a general trend towards higher activity with increasing water content in the material preparation system. This is complicated by some irregularities in the data from the samples prepared from solvents with roughly comparable water ethanol volume ratios. While many systems have been described where the catalytic activity correlates with changes in textural properties[9], the trends in activity found in this study correlate best with an increase in framework mesopore diameter, and do not follow the... 

Influence of Ethanol. Three different amorphous aluminosilicate solids of Si/Al ratios 1.33, 1.48 and 4.28 were synthesized by mixing sodium silicate and aluminate solutions of various concentrations. These solids were extensively ion-exchanged with LiCl and NaCl solutions. The lithium and sodium containing solids (2g) were then mixed with 50 mL of 1JJ LiOH and NaOH, respectively. The hydroxide solutions contained 0%, 10%, 25%, 50% and 75% ethanol (volume by volume). These samples were then heated to 90-95 C, and formation of zeolites was monitored by powder diffraction. In one experiment, the lithium aluminosilicate solid was reacted in the NaOH system. 

Figure 3. X-ray diffraction patterns as a function of ethanol content for 2g Na aluminosilicate (Si/Al - 1.33) in 50 mL of 1M NaOH with varying ethanol content. From top 0%, 10%, 25%, 50% and 75% ethanol (volume percent). X-ray patterns taken -8 hours after reaction at 90-95°C. The intensity axis is the same for all the patterns.

Add 10 ml cold ethanol (volume may vary) to the brown solution and place in an ice bath. Filter the cold solution using a Hirsh funnel. Collect the precipitate and repeat this procedure. 

Table 4.7 Ethanol volume % versus specific gravity at 15 °C...

Figure 10.8. Evolution of the water contact angle of the modified PHBHVfilms for different irradiation times, a) PHBHV-g-PMETA film ([META]=3M, butan-2-one/water/edumol volume ratio 10/10/10), b) PHBHV-g-PHEMA film ([HEMA]=4M, butan-2-one/water/ethanol volume ratio 10/80/10) and c) PHBHV-g-PMESA film ([MESA] = IM with butan-2-one/water/ethanol volume ratio 10/10/10). Reprinted (adapted) with permission from [MAN 14]...

Bakal et al. [7] described a variation of the balloon occlusion technique. They performed all renal embolizations during selective placement of an occlusion balloon catheter in the distal main renal artery. Estimates of ethanol volume needed for embolization were made by test injecting contrast material during balloon occlusion. After infusion of the ethanol, the balloon was left inflated for 5 min. As the balloon was deflating, gentle suction through the distal endhole of the catheter prevented reflux of... 

If wine is not sulfited after malolactic fermentation, bacteria continue to survive for months. Carre (1982) observed a small decrease from 10 UFC/ml to 10 UFC/ml after 6 months of conservation in a wine stored at 19°C with a pH of 3.9 and an ethanol volume of 11.25%. Sulfiting immediately after the end of malolactic fermentation is intended to accelerate this death phase. No significant viable population should be left in the wine. Even if they can no longer multiply very actively. 

Relative silane concentration versus time during acid- and base-catalyzed hydrolysis of different silanes in ethanol (volume ratio silane to EtOH = 1 1). (CH3)jSiOCjH5. V (CHjljSKOCjHj) . CHjSKOCjHj),. O Si(OC2Hj)4. A Si(OCHj)4 [61]. 

Fig. 9.2 SEM images of Cep3 prepared in different ethanol volumes 2 mL (a) 3 mL (b) (Reprinted with the permission from Ref [6]. Copyright 2008 American Chemical Society)...

Example 3.4.3 Schaetzel et al. (2004) have studied the per-vaporation of a water-ethanol mixture through a polyvinylalcohol based membrane as a function of feed water concentration at 60 °C. They have also measured the equilibrium volume fraction of water and ethanol in the membrane for such feed mixtures. When there is very high vacuum in the permeate side, it is possible to correlate the water flux (mol/m -s) with the feed side water and ethanol volume fractions CaHjOH.mlo- respectively,... 

Kbrklsch, et al. have separated uranium from tungsten 19 means of anion exchange. The uranium Is adsorbed on Dowex-3. resin from a solution containing 20 4h HCl and 80 ethanol (volume ft). Ascorbic acid Is used to reduce siny Iron present. The resin Is washed with a similar solution and uranium Is eluted with an ether-saturated 0.3M HCl solution. No tungsten la observed In the final eluate. 

Hydrolysis of />-Tolunitrile. As in the case of benzonitrile, alkaline h> drolysis is preferable to hydrolysis by 70% sulphuric acid. Boil a mixture of 5 g. of p-tolunitrile, 75 ml. of 10% aqueous sodium hydroxide solution and 15 ml. of ethanol under a reflux water-condenser. The ethanol is added partly to increase the speed of the hydrolysis, but in particular to prevent the nitrile (which volatilises in the steam) from actually crystallising in the condenser. The solution becomes clear after about i hour s heating, but the boiling should be continued for a total period of 1-5 hours to ensure complete hydrolysis. Then precipitate and isolate the p-toluic acid, CH3CgH4COOH, in precisely the same way as the benzoic acid in the above hydrolysis of benzonitrile. Yield 5 5 g. (almost theoretical). The p-toluic acid has m.p. 178°, and may be recrystallised from a mixture of equal volumes of water and rectified spirit. 

Prepare a mixture of 30 ml, of aniline, 8 g. of o-chloro-benzoic acid, 8 g. of anhydrous potassium carbonate and 0 4 g. of copper oxide in a 500 ml. round-bottomed flask fitted with an air-condenser, and then boil the mixture under reflux for 1 5 hours the mixture tends to foam during the earlier part of the heating owing to the evolution of carbon dioxide, and hence the large flask is used. When the heating has been completed, fit the flask with a steam-distillation head, and stcam-distil the crude product until all the excess of aniline has been removed. The residual solution now contains the potassium. V-phenylanthrani-late add ca. 2 g. of animal charcoal to this solution, boil for about 5 minutes, and filter hot. Add dilute hydrochloric acid (1 1 by volume) to the filtrate until no further precipitation occurs, and then cool in ice-water with stirring. Filter otT the. V-phcnylanthranilic acid at the pump, wash with water, drain and dry. Yield, 9-9 5 g. I he acid may be recrystallised from aqueous ethanol, or methylated spirit, with addition of charcoal if necessary, and is obtained as colourless crystals, m.p. 185-186°. 

Finally, add an excess of concentrated hydrochloric acid slowly with stirring to the alkaline filtrate remaining from the original reaction product. As the solution becomes acid, the sulphonyl-aniline separates as a thick sticky syrup which, when stirred, rapidly crystallises. Cool the mixture in ice-water if necessary, and then filter off the solid product at the pump, wash well with water, and drain. Recrystallise from a mixture of 2 volumes of ethanol and i volume of water to prevent the sulphonyl-aniline from separating as an emulsion, allow the hot solution to cool spontaneously (with occasional stirring) until crystallisation starts, and... 

Dissolve 10 g. of chloro- 2,4-dinitrobenzenet in 50 ml. of dioxan in a 250 ml. conical flask. Dilute 8 ml. of hydrazine hydrate with an equal volume of water and add this slowly with shaking to the dioxan solution, keeping the temperature between zo " and 25°. Heat under reflux for 10 minutes to complete the reaction and then add 5 ml. of ethanol and heat again for 5 minutes. Cool and filter oflF the orange 2,4-dinitrophenylhydra-zine. Recrystallise the dry product from ethyl acetate m.p. 200° (decomp.). Yield, 7 g. 

Dinitrophenylhydra2ones usually separate in well-formed crystals. These can be filtered at the pump, washed with a diluted sample of the acid in the reagent used, then with water, and then (when the solubility allows) with a small quantity of ethanol the dried specimen is then usually pure. It should, however, be recrystallised from a suitable solvent, a process which can usually be carried out with the dinitrophenylhydrazones of the simpler aldehydes and ketones. Many other hydrazones have a very low solubility in most solvents, and a recrystallisation which involves prolonged boiling with a large volume of solvent may be accompanied by partial decomposition, and with the ultimate deposition of a sample less pure than the above washed, dried and unrecrystal-lised sample. 

Mix 6 2 ml. (6 4 g.) of pure ethyl acetoacetate and 5 ml. of pure phenylhydrazine in an evaporating-basin of about 75 ml. capacity, add 0 5 ml. of acetic acid and then heat the mixture on a briskly boiling water-bath (preferably in a fume-cupboard) for I hour, occasionally stirring the mixture with a short glass rod. Then allow the heavy yellow syrup to cool somewhat, add 30-40 ml. of ether, and stir the mixture vigorously the syrup may now dissolve and the solution shortly afterwards deposit the crystalline pyrazolone, or at lower temperatures the syrup may solidify directly. Note. If the laboratory has been inoculated by previous preparations, the syrup may solidify whilst still on the water-bath in this case the solid product when cold must be chipped out of the basin, and ground in a mortar with the ether.) Now filter the product at the pump, and wash the solid material thoroughly with ether. Recrystallise the product from a small quantity of a mixture of equal volumes of water and ethanol. The methyl-phenyl-pyrazolone is obtained... 

Gently warm a mixture of 32 g. (32 ml.) of ethyl acetoacetate and 10 g. of aldehyde-ammonia in a 400 ml. beaker by direct heating on a gauze, stirring the mixture carefully with a thermometer. As soon as the reaction starts, remove the heating, and replace it when the reaction slackens, but do not allow the temperature of the mixture to exceed 100-no the reaction is rapidly completed. Add to the mixture about twice its volume of 2A -hydrochloric acid, and stir the mass until the deposit either becomes solid or forms a thick paste, according to the quality of the aldehyde-ammonia employed. Decant the aqueous acid layer, repeat the extraction of the deposit with more acid, and again decant the acid, or filter off the deposit if it is solid. Transfer the deposit to a conical flask and recrystallise it twice from ethanol (or methylated spirit) diluted with an equal volume of water. The i,4-dihydro-collidine-3,5-dicarboxylic diethyl ester (I) is obtained as colourless crystals, m.p. 130-131°. Yield 12 5 g,... 

Collidine 2i5 d carboxylic acid. Boil a mixture of 5 g. of the ester (II) and 50 ml. of 15% ethanolic potash under reflux for 30 minutes. The dipotassium salt crystallises during the boiling and during the subsequent cooling. Filter off the potassium salt at the pump and wash it with a small quantity of ethanol. Dilute the filtrate with about an equal volume of ether to precipitate a further small crop of the salt. Yield of combined crops 4 5 g. from 5 g. of the estei (I). 

The arsinic acid thus obtained is of high quality after draining, however, it can be directly recrystallised from ethanol or from a large volume of hot water m.p. of recrystallised acid, 205-206°. 

For the preparation of 2 4-dinitrophenylhydrazones, dissolve the carbonyl compound (say, 0-5 g.) in 5 ml. of ethanol and add the cal culated volume of the reagent. If a precipitate does not form immediately, dilute with a little water. Collect the derivative and recrystalhse it as above. 

The sulphonanilldes may be prepared by either of the following methods —(i) Reflux the solution of the sulphonyl chloride in benzene obtained as above, with 2 5 g. of aniline for 1 hour. Concentrate the benzene solution to half its volume and cool in ice. Collect the solid which separates on a filter, wash with hot water, and recrystallise from ethanol or dilute ethanol. 

Dissolve 1 g. of the sulphonic acid or its sodium salt in the minimum volume of boiling water and add a saturated aqueous solution of 1 g. of p-toluidine hydrochloride. Cool, Alter off the precipitate of the p-tolu-idine salt, and recrystallise it from hot water or from dilute ethanol. 

Dissolve 1 g. (or 0 01 mol) of the phenol in a solution of 0-40 g. of sodium hydroxide in 5 ml. of water. Add the resulting solution to 2-Og. of 2 4-dinitrochlorobenzene dissolved in 30 ml. of 95 per cent, ethanol add more alcohol, if necessary, to effect solution. Heat the solution under reflux on a water bath until the colour (usually red) is discharged and a copious precipitate of sodium chloride appears (30-60 minutes). Dilute the reaction mixture with an equal volume of water, filter off the precipitated 2 4-dinitrophenyl ether, wash with water, and recrystallise from alcohol. 

The diethyl fumarate is readily prepared as follows. Reflux a mixture of 146 g. of fumaric acid (Section 111,143), 185 g. (236 ml.) of absolute ethanol, 450 ml. of boizene and 20 g. of concentrated sulphuric acid for 12 hours. Pour into a large volume of water, separate the benzene layer, wash successively with water, saturated lodium bicarbonate solution and water, dry with anhydrous magnesium sulphate, and remove the solvent on a steam bath. Distil the residue and collect the diethyl fumarate at 213-215° the yield is 150 g. 

Method B. Place 125 g. (106 -5 ml.) of diethyl phthalate and 25 g. of molecular sodium (sodium sand see Section 11,50,6) in a 500 ml. round-bottomed flask fitted with a reflux condenser and dropping funnel. Heat the flask on a steam bath and add a mixture of 122 5 g. (136 ml.) of dry ethyl acetate and 2 5 ml. of absolute ethanol over a period of 90 minutes. Continue the heating for 6 hours, cool and add 50 ml. of ether. Filter the sodium salt (VI) on a sintered glass funnel and wash it with the minimum volume of ether. Dissolve the sodium salt (96 g.) in 1400 ml. of hot water in a 3-htre beaker, cool the solution to 70°, stir vigorously and add 100 ml. of sulphuric acid (3 parts of concentrated acid to 1 part of... 

Prepare a saturated solutiotr of sodium bisulfite at the laboratory temperature from 40g of finely powdered sodium bisulphite about 70ml. of water are required. Measure the volume of the resulting solution and treat it with 70 per cent, of its volume of rectified spirit (or methylated spirit) [ethanol or methanol or both, dude] add sufficient water (about 45mL.) to just dissolve the precipitate which separates. ... 

METHOD 2 [89]--1M MDA or benzedrine and 1M benzaldehyde is dissolved in 95% ethanol (Everclear), stirred, the solvent removed by distillation then the oil vacuum distilled to give 95% yellow oil which is a Schiff base intermediate. 1M of this intermediate, plus 1M iodomethane, is sealed in a pipe bomb that s dumped in boiling water for 5 hours giving an orangy-red heavy oil. The oil is taken up in methanol, 1/8 its volume of dH20 is added and the solution refluxed for 30 minutes. Next, an equal volume of water is added and the whole solution boiled openly until no more odor of benzaldehyde is detected (smells like almond extract). The solution is acidified with acetic acid, washed with ether (discard ether), the MDMA or meth freebase liberated with NaOH and extracted with ether to afford a yield of 90% for meth and 65% for MDMA. That s not a bad conversion but what s with having to use benzaldehyde (a List chemical) Strike wonders if another aldehyde can substitute. 

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