Acids diluting

Anhydrous titanium dioxide is only soluble with difficulty in hot concentrated sulphuric acid dilution allows the crystallisation of a sulphate of formula T10S04.H20, but it is doubtful if the titanyl cation TiO actually exists, either in solution or the solid. Certainly [TifHjOIn] does not exist, and solutions of titanyl salts may best be considered to contain ions [Ti(0H)2(H204)] . Titanium... 

E values. Nitric acid attacks mercury, oxidising it to Hg (aq) when the acid is concentrated and in excess, and to Hgf (aq) when mercury is in excess and the acid dilute. Hydriodic acid Hl(aq) attacks mercury, because mercury(Il) readily forms iodo-complexes (see below, p. 438). 

Meanwhile assemble the apparatus shown in Fig. 62, or that in Fig. 23(D), p. 45, having a distilling-flask of at least 500 ml. capacity in either case. If an ordinary condenser C (Fig. 62) is employed, fit the lower end of the condenser by means of a short piece of rubber tubing to a small inverted funnel. Arrange the latter so that its lip is just below the surface of 25 ml. of concentrated hydrochloric acid diluted with 75 ml. of water contained in a 250 ml. beaker B the hydro-. chloric acid is thereby prevented from being sucked back into the... 

SULPHANILAMIDE. (Reaction C.) Add 15 g. of the above thoroughly drained sulphonamide to 10 ml. of concentrated hydrochloric acid diluted with 20 ml. water, and boil the mixture gently under reflux for i hour. Then add 30 ml. of water and heat the mixture again to boiling, with the addition of a small quantity of animal charcoal. Filter the boiling solution, and add powdered sodium carbonate in small quantities to the filtrate with stirring until all eflFervescence ceases and the sulphanilamide is precipitated as a white powder. Cool the mixture thoroughly and filter oflF the sulphanilamide at the pump, wash with water and dry. Yield, ca. 10 g. 

For dehydrogenation, add this ester to dilute nitric acid (20 ml. of the concentrated acid diluted with 40 ml. of water) and boil the mixture under reflux for about 5 minutes, during which the ester gently efferv esces and Anally gives a clear solution. Cool this solution in ice-w ater, make alkaline with aqueous sodium carbonate solution and extract tw ice with ether (50 ml. for each extraction). Dry the extract with sodium sulphate, filter, and then distil using a small distilling-flask... 

Dissolve 13 g. of sodium in 30 ml. of absolute ethanol in a 250 ml. flask carrying a reflux condenser, then add 10 g. (9 5 ml.) of redistilled ethyl malonate, and place the flask on a boiling water-bath. Without delay, add a solution of 5 3 g. of thiourea in a minimum of boiling absolute ethanol (about 100 ml.). The sodium salt of thiobarbituric acid rapidly begins to separate. Fit the water-condenser with a calcium chloride guard-tube (Fig. 61, p. 105), and boil the mixture on the water-bath for 1 hour. Cool the mixture, filter off the sodium salt at the pump and wash it with a small quantity of cold acetone. Dissolve the salt in warm water and liberate the acid by the addition of 30 ml. of concentrated hydrochloric acid diluted with 30 ml. of water. Cool the mixture, filter off the thiobarbituric acid, and recrystallise it from hot water. Colourless crystals, m.p. 245 with decomposition (immersed at 230°). Yield, 3 5 -4 0 g. 

At the end of about an hour,f filter the solution and tfansfer 20 ml. of the clear filtrate to a boiling-tube. Dissolve 2 5 ml. of phenylhydrazine in 3 ml. of glacial acetic acid diluted with 3 ml. of water, and add this solution to that in the boiling-tube. Mix well and place the tube in a boiling water-bath. After about 15 minutes, crystals of glucosazone begin to separate. At the end of about i hour, filter off the precipitate and identify (p. 319). 

Acetic Acid, Dilute. Approv. 4/I/, Dilute 230 ml. of glacial acetic acid with water until total volume is i litre. 

Hydrochloric Acid, Dilute, i vol. of cone. HCl to 3 vols. of water. 

I) An alternative procedure is to cool the solution containing the sodium sul. phanilate and sodium nitrite in a bath of crushed ice to about 5° and then add 10-5 ml. of concentrated hydrochloric acid diluted with an equal volume of water slowly and with stirring the temperature must not be allowed to rise above 10 and an excess of nitrous acid should be present (the solution is tested after standing for 5 minutes). The subsequent stages in the preparation—addition of dimethyl-aniline solution, etc.—are as above. 

Dissolve 5 g. of finely-powdered diazoaminobenzene (Section IV,81) in 12-15 g. of aniline in a small flask and add 2-5 g. of finely-powdered aniline hydrochloride (1). Warm the mixture, with frequent shaking, on a water bath at 40-45° for 1 hour. Allow the reaction mixture to stand for 30 minutes. Then add 15 ml. of glacial acetic acid diluted with an equal volume of water stir or shake the mixture in order to remove the excess of anihne in the form of its soluble acetate. Allow the mixture to stand, with frequent shaking, for 15 minutes filter the amino-azobenzene at the pump, wash with a little water, and dry upon filter paper Recrystallise the crude p-amino-azobenzene (3-5 g. m.p. 120°) from 15-20 ml. of carbon tetrachloride to obtain the pure compound, m.p. 125°. Alternatively, the compound may be recrystaUised from dilute alcohol, to which a few drops of concentrated ammonia solution have been added. 

Method 2 (from the free amine). Dissolve 9 - 3 g. (9 1 ml.) of aniline in 10 ml. of glacial acetic acid diluted to 100 ml. contained in a 250 ml. beaker or conical flask, and add with stirring or shaking a solution of 6 5 g. of pure sodium cyanate in 50 ml. of warm water. Allow to stand for 30 minutes, then cool in ice, and allow to stand for a further 30 minutes. Filter at the pump, wash with water and dry in the steam oven. The resulting phenylurea is generally colourless and has a m.p. of 148° (i.e., is pure) the yield is 11 g. If the colour or the m.p. of the product is not quite satisfactory, recrj stallise it from boiling water (10 ml. per gram) as in Method 1. 

Commercial o-clilorobenzoic acid may be purified in the following niannor. Dissolve 60 g. of the technical acid in 200 ml. of hot water containing 20 g. of sodium carbonate, d 10 g. of decolourising carbon, boil for 15 minutes, and filter at the pump. Add the filtrate with stirring to 31 ml. of concentrated hydrochloric acid diluted with an equal volume of water. Collect the purified acid with suction, wash it with a little cold water, and dry at 100°. 

Acids including oxalic acid). Dilute by drinking much water, followed by lime water or milk of magnesia. Milk may then be given but no emetics. 

Ceric sulfate, O.IA Ce(lV) to Ce(lll). Dissolve 63.26 g of cerium(lV) ammonium sulfate dihydrate in 500 mL of 2N sulfuric acid. Dilute the solution to 1 L and standardize against the... 

Table 4. Plant Corrosion Test in Sulfuric Acid Dilution with Recirculated Phosphoric Acid ...

They show good to excellent resistance to highly aromatic solvents, polar solvents, water and salt solutions, aqueous acids, dilute alkaline solutions, oxidative environments, amines, and methyl alcohol. Care must be taken in choice of proper gum and compound. Hexafluoropropylene-containing polymers are not recommended for use in contact with ammonia, strong caustic (50% sodium hydroxide above 70°C), and certain polar solvents such as methyl ethyl ketone and low molecular weight esters. However, perfluoroelastomers can withstand these fluids. Propylene-containing fluorocarbon polymers can tolerate strong caustic. 

Resin cured butyl (HR) Acids Lyes Strong alkahes Strong phosphoric acid Dilute mineral acids Ketones Amines Water Fats and fatty acids Petroleum oils Chlorinated hydrocarbons Liquids with dissolved chlorine Mineral oil Oxygen rich demin. water Strong oxidants... 

C. Thymoquinone.—The wet aminothymol thus prepared is immediately dissolved in no cc. of concentrated sulfuric acid diluted to 4 1. and contained in a 12-I. flask. To this solution is added 150 g. of sodium nitrite (2.18 moles), in 5-10-g. portions, with shaking after each addition. The resulting mixture is heated to 60° on a steam bath, with occasional shaking, for half an hour (Note 5), and is then distilled in a current of steam, by means of the apparatus described in Org. Syn. 2, 80 (Note 6). All the thymoquinone passes over with the first 3 1. of distillate it solidifies on cooling, and is filtered with suction (Note 7), washed, and dried at room temperature. The yield is 80-87 g. (73-80 per cent of the theoretical amount) of bright yellow crystals, melting at 43-45° (Note 8). 

The solution containing sodium malate is neutralized with acetic acid, diluted to contain about 5 per cent of sodium... 

The residue (12 g) which contains the 18-iodo-18,20-ether is dissolved in 200 ml of acetone, 5 g of silver chromate is added Note 3) and after cooling to 0°, 11.8 ml of a solution of 13.3 g of chromium trioxide and 11.5 ml of concentrated sulfuric acid, diluted to 50 ml with water is added during a period of 5 min. After an additional 60 min, a solution of 112 g of sodium acetate in 200 ml of water is added and the mixture diluted with benzene (400 ml), filtered and the benzene layer separated. The aqueous phase is reextracted with benzene, washed with half-saturated sodium chloride solution, dried and evaporated to yield 11.2 g of a crystalline residue. Recrystallization from ether gives 7.2 g (72%) of pure 3/5, 1 la, 20/5-trihydroxy-5a-pregnan-18-oic acid 18,20 lactone 3,11-diacetate mp 216-218°. 

Reaction.—Dissolve a diop of phenylhydrazine in two diojis of glacial acetic acid, dilute with about i c.c. of water, and acid a diop of pyruvic acid. A yellow crystalline piecipitate of tlio phen)Ihydrazone, CH3.C (N.NH.C(,H5).CO.OH, is formed. 

Add to a few drops of phenylhydrazine an equal quantity of glacial acetic acid, dilute with a little water, and Reid a... 

To the cooled solution is added dropwise with stirring, a solution of 64 g (0.48 mole) of -amyl nitrate in 100 ml of dry tetrahydrofuran during a period of 1 hour. The solution is finally allowed to warm to room temperature overnight. Work-up is carried out by adding an excess of ice-acetic acid, diluting with water, and extracting the aqueous solution several times with ether. The ether extracts are washed thoroughly... 

Into a stirred, cooled (10°-15°C) solution of 26.2 grams (0.1 mol) of 2-amino-5-chlorobenzo-phenone (3-oxime in 150 ml of dioxane were introduced in small portions 12.4 grams (0.11 mol) of chloracetyl chloride and an equivalent amount of 3 N sodium hydroxide. The chlor acetyl chloride and sodium hydroxide were introduced alternately at such a rate so as to keep the temperature below 15°C and the mixture neutral or slightly alkaline. The reaction was completed after 30 minutes. The mixture was slightly acidified with hydrochloric acid, diluted with water and extracted with ether. The ether extract was dried and concentrated in vacuo. Upon the addition of ether to the oily residue, the product, 2-chloroacetamido-5-chlorobenzophenone (3-oxime, crystallized in colorless prisms melting at 161°-162°C. 

To a solution of 93.8 g of the monoglycol ester in 500 ml of benzene, there are added 55 g of nicotinic acid chloride and 25 g of trimethylemine dissolved in 200 ml of benzene. The solution is stirred gently at a temperature of 60°C for two hours. After this time, the solution is cooled and washed successively with water, dilute hydrochloric acid, dilute ammonia and water until neutrality, it is dried over anhydrous sodium sulfate, and the sol vent Is evaporated under vacuum In this wey llOg of glycol 2-(p-chlorophenoxy)-2-methylpropionate nico-tlnate Is prepared, which represents a yield of 84%. The product is a sllghly yellow oil having a refraction index of no = 1.5422 and which is distilled with decomposition et 214°C at a pressure of 0.3 mm. 

Organic acids Dilute solutions of organic acids, especially if well aerated, attack cast iron at uneconomical rates. Temperature and velocity are also accelerating factors. 

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