Benzene volume

Hamster urine (dichlorobenzidine, mono- and di-acetyldichloroben-zidine, conjugates) Adjustment of pH, extraction with benzene, volume reduction, formation of heptafluorbutyryl derivatives for conjugates alkaline hydrolysis of aqueous phase followed by derivatization as above. GC/ECD 7-48 g/L No data Bowman and Nony1981 Nony and Bowman 1980 Nony et al. 1980... 

A solution of amino ketone 11 (20 g) in benzene (1 L) was irradiated with a 500-W Hg lamp and the conversion monitored by TLC. The benzene volume was then reduced to about 250 mL and extracted with cold 1% HC1 (5x). The aqueous solution was washed thoroughly with Et20 and rendered alkaline by addition of 2% NaOH. The oily precipitate formed was decanted and dissolved in El20. This solution was dried (Na2S04), evaporated and the residue crystallized (i-PrOH). 

Air (CDDs) Drawing of approximately 325 m3 of air through quartz fiber filter/polyurethane foam Soxhlet extraction with benzene, volume reduction clean-up using silica, alumina, activated carbon volume reduction addition of [13C12]2,3,7,8-TCDD. HRGC/HRMS MID (EPA TO-9) 1-5 pg/m3 68-140 from ultra pure, filtered air EPA1988g... 

Figure 13. Three-dimensional conductance-benzene volume-cetyl alcohol concentration plot calculated using Equation 2 for conductometric titration at 63°C of 25 cc water containing 0.15 g hexadecyltrimethylammonium bromide and varying concentrations of cetyl alcohol with benzene at a constant rate of 1 cc/min viewed at a horizontal angle of 250° and a vertical angle of 65°.

Figure 13. Opening of the interlameUar space. Enthalpy of displacement (A12H) and basal spacing (dn) at different benzene volume fraction ( 2) in the adsorption layer. System hexadecylammonium-vermiculite in methanol(l)- -benzene(2) mixture.

Figure 2. Plot of benzene flux vs. benzene volume fraction in the feed solution for a PVA-AgNOa membrane (7% Ag by mass) crosslinked with formsddehyde as described in reference 8. The membrane thickness was approximately ISO pm.

For cyclic compounds, it is necessary to reduce the volume obtained by 0.0183 m /kmol. For example, benzene has a volume of diffusion of ... 

Among the compounds susceptible to evaporation, particular attention is focused on benzene. In the two conditions indicated above, for equal benzene contents in the fuel (1.5% volume), the benzene evaporative losses are reduced by 21% and 11%, respectively, when the vapor pressure decreases by 1 psi, that is, 69 mbar. 

A European Directive, 85/210/EEC, limits benzene content to 5% by volume in all gasolines regular, premium, with or without lead. This level is easily achieved, since the average value in 1993 was less than 3%. in France, for example, average benzene concentrations of 1.7% and 2.6% were reported for leaded and unleaded premium fuels, respectively, in 1993. 

Why is potassium aluminium sulphate not soluble in benzene A compound M has the composition C = 50.0% H=12.5%o A1 = 37.5%. 0.360 g of M reacts with an excess of water to evolve 0.336 1 of gas N and leave a white gelatinous precipitate R. R dissolves in aqueous sodium hydroxide and in hydrochloric acid. 20 cm of N require 40 cm of oxygen for complete combustion, carbon dioxide and water being the only products. Identify compounds N and R, suggest a structural formula for M, and write an equation for the reaction of M with water. (All gas volumes were measured at s.t.p.)... 

Experiment 6. Fractional Distillation of a Mixture of Benzene and Toluene. Fractionally distil about 40 ml. of a mixture of equal volumes of benzene and toluene, using the type of fractionating column shown in Fig. ii(b), in which about 18-20 cm. of the column are actually filled with glass sections, but in which the cotton-wool lagging is not used. Distil very slowlyy so that the total distillation occupies about hours. Shield the apparatus very carefully from draughts. Collect the fractions having the b.ps (a) 80-85°, ( ) 85-107°, (c) 107-111°. A sharp separation should be obtained, e.g.y these fractions should have volumes of about 19, 2, and 17 ml. respectively. 

Hence one extraction with 100 ml. of benzene removes 3 0 g. (or 75 per cent.) of the n-butyric acid, whilst three extractions remove 3 5 g. (or 87-5 per cent.) of the total acid. This clearly shows the greater efficiency of extraction obtainable with several extractions when the total volume of solvent is the same. Moreover, the smaller the distribution coefficient between the organic solvent and the water, the larger the number of extractions that will be necessary. 

Place 100 g. of adipic acid in a 750 ml. round-bottomed flask and add successively 100 g. (127 ml.) of absolute ethyl alcohol, 250 ml. of sodium-dried benzene and 40 g. (22 ml.) of concentrated sulphuric acid (the last-named cautiously and with gentle swirling of the contents of the flask). Attach a reflux condenser and reflux the mixture gently for 5-6 hours. Pour the reaction mixture into excess of water (2-3 volumes), separate the benzene layer (1), wash it with saturated sodium bicarbonate solution until eflfervescence ceases, then with water, and dry with anhydrous magnesium or calcium sulphate. Remove most of the benzene by distillation under normal pressure until the temperature rises to 100° using the apparatus of Fig. II, 13, 4 but substituting a 250 ml. Claisen flask for the distilling flask then distil under reduced pressure and collect the ethyl adipate at 134-135°/17 mm. The yield is 130 g. 

The acetamide often contains a minute amount of impurity having an odour resembling mice excrement this can be removed by washing with a small volume of a 10 per cent, solution of ethyl alcohol in ether or by recrystallLsation. Dissolve 5 g. of impure acetamide in a mixture of 5 ml. of benzene and 1 5 ml. of dry ethyl acetate warm on a water bath until all is dissolved and cool rapidly in ice or cold water. Filter oflF the crystals, press between Alter paper and dry in a desiccator. The unpleasant odour is absent and the pure acetamide melts at 81°. Beautiful large crystals may be obtained by dissolving the acetamide (5 g.) in warm methyl alcohol (4 ml.), adding ether (40 ml.) and allowing to stand. 

Dissolve 57 g. of dry malonic acid in 92 5 ml. of dry P3rridine contained in a 500 ml. round-bottomed flask, cool the solution in ice, and add 57 g. (70 ml.) of freshly distilled n-heptaldehyde (oenanthol) with stirring or vigorous shaking. After a part of the aldehyde has been added, the mixture rapidly seta to a mass of crystals. Insert a cotton wool (or calcium chloride) tube into the mouth of the flask and allow the mixture to stand at room temperature for 60 hours with frequent shaking. Finally, warm the mixture on a water bath until the evolution of carbon dioxide ceases (about 8 hours) and then pour into an equal volume of water. Separate the oily layer and shake it with 150 ml. of 25 per cent hydrochloric acid to remove pyridine. Dissolve the product in benzene, wash with water, dry with anhydrous magnesium sulphate, and distil under reduced pressure. Collect the ap-nonenoic acid at 130-13272 mm. The yield is 62 g. 

Commercial benzene may be purified by shaking repeatedly with 10 per cent, of its volume of concentrated sulphuric acid until the acid layer is almost colourless, then washing successively with cold water, 10 per cent, sodium carbonate solution and water, and drying with anhydrous calcium chloride or inagnosiuin sulphate. Distillation then yields pure benzene. 

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. 

Hydrolysis of p-tolunitrile to p-toluic acid. Boil a mixture of 5 g. of p-tolunitrile, 80 ml. of 10 per cent, aqueous sodium hydroxide solution and 15 ml. of alcohol under a reflux condenser. (The alcohol is added to prevent the nitrile, which volatUises in the steam, from crystalhsing in the condenser it also increases the speed of hydrolysis. The alcohol may be omitted in the hydrolysis of nitriles which are hquid at the ordinary temperature, e.g., benzo-nitrUe.) The solution becomes clear after heating for about 1 hour, but continue the boiling for a total period of 1 - 5 hours to ensure complete hydrolysis. Detach the condenser and boil the solution for a few minutes in the open flask to remove dissolved ammonia and incidentally some of the alcohol CAUTION /). Cool, and add concentrated hydrochloric acid until precipitation of the p-toluic acid is complete. When cold, filter off the p-toluic acid with suction and wash with a little cold water. Recrystallise from a mixture of equal volumes of water and alcohol (methylated spirit) or from benzene. The yield of p-toluic acid, m.p. 178°, is 5-5 g. 

Dissolve 2-3 g. of methyl p-toluenesnlphonate in 10 ml. of dry benzene, add 1 g. of the amine, and boU the mixture for 20-30 minutes. Cool, and filter the precipitated quaternary salt. Recrystallise by dissolving the solid in the minimum volume of boiling ethyl alcohol and then adding ethyl acetate until crystallisation commences. Filter the cold mixture, dry rapidly on a porous plate, and determine the m.p. immediately. 

Oximes (compare Section III,74,B). The following procedure has wide application. Dissolve 0-5 g. of hydroxylamine hydrochloride in 2 ml. of water, add 2 ml. of 10 per cent, sodium hydroxide solution and 0-2 g. of the aldehyde (or ketone). If the latter is insoluble, add just sufficient alcohol to the mixture to give a clear solution. Heat the mixture under reflux for 10-15 minutes, and then cool in ice. If crystals separate, filter these off, and recrystallise from alcohol, dilute alcohol, benzene or light petroleum (b.p. 60-80°). If no solid separates on cooling, dilute with 2-3 volumes of water, filter the precipitated sohd, and recrystallise. 

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