Turbidance

Nessler tubes Cylinders of thin glass, generally graduated, used for comparing turbidities and colours of solutions. 

Foam rheology has been a challenging area of research of interest for the yield behavior and stick-slip flow behavior (see the review by Kraynik [229]). Recent studies by Durian and co-workers combine simulations [230] and a dynamic light scattering technique suited to turbid systems [231], diffusing wave spectroscopy (DWS), to characterize coarsening and shear-induced rearrangements in foams. The dynamics follow stick-slip behavior similar to that found in earthquake faults and friction (see Section XU-2D). 

The action of concentrated sulphuric acid liberates hydrogen fluoride, which attacks glass, forming silicon tetrafluoride the latter is hydrolysed to silicic acid by water, which therefore becomes turbid,... 

Dissolve 5 g. of aniline hydrochloride in 120 ml. of hot water contained in a 200 ml. conical flask and then add 4 g. of potassium cyanate. Heat the solution on a water-bath for 30 minutes, adding about 1-2 g. of animal charcoal towards the end of the heating if a slight turbidity has developed. Now bring the solution quickly to the boil over a gauze, and filter it at the pump, using a Buchner funnel and flask which have been preheated by the filtration of some boiling distilled water. The clear... 

For ethyl alcohol, two volumes of dicycZohexyl are mixed with one volume of the alcohol, a thermometer is introduced, and the mixture heated until it becomes clear. The solution is then slowly cooled, with constant stirring, and the temperature is determined at which the opalescent solution suddenly becomes turbid so that the immersed portion of the mercury thread of the thermometer is no longer clearly visible. This is the C.S.T. The water content may then be evaluated by reference to the following table. 

If the substance is found to be far too soluble in one solvent and much too insoluble in another solvent to allow of satisfactory recrystallisation, mixed solvents or solvent pairs may frequently be used with excellent results. The two solvents must, of course, be completely miscible. Recrystallisation from mixed solvents is carried out near the boiling point of the solvent. The compound is dissolved in the solvent in which it is very soluble, and the hot solvent, in which the substance is only sparingly soluble, is added cautiously until a slight turbidity is produced. The turbidity is then just cleared by the addition of a small quantity of the first solvent and the mixture is allowed to cool to room temperature crystals will separate. Pairs of liquids which may be used include alcohol and water alcohol and benzene benzene and petroleum ether acetone and petroleum ether glacial acetic acid and water. 

If a turbid solution is obtained, suggesting the presence of a secondary alcohol but not excluding a tertiary alcohol, a further test with concentrated hydrochloric acid must be made. Mix 1 ml. of the alcohol with 6 ml. of concentrated hydrochloric acid, and observe the result —... 

Allyl Chloride. Comparatively poor yields are obtained by the zinc chloride - hydrochloric acid method, but the following procedure, which employs cuprous chloride as a catalyst, gives a yield of over 90 per cent. Place 100 ml. of allyl alcohol (Section 111,140), 150 ml. of concentrated hydrochloric acid and 2 g. of freshly prepared cuprous chloride (Section II,50,i one tenth scale) in a 750 ml. round-bottomed flask equipped with a reflux condenser. Cool the flask in ice and add 50 ml. of concen trated sulphuric acid dropwise through the condenser with frequent shaking of the flask. A little hydrogen chloride may be evolved towards the end of the reaction. Allow the turbid liquid to stand for 30 minutes in order to complete the separation of the allyl chloride. Remove the upper layer, wash it with twice its volume of water, and dry over anhydrous calcium chloride. Distil the allyl chloride passes over at 46-47°. 

To prepare the anhydride , boil a solution of 01 g. of the dimedone derivative (I) in 5 ml. of 80 per cent, ethanol to which 1 drop of concentrated hydrochloric. acid has been added for 5 minutes, than add hot water until the mixture is just turbid, cool and collect the anhydride by filtration. Recrystallise it from dilute methanol. 

Prepare a solution of phenylhydrazine by dissolving 1 0 g. of phenyl-hydrazine hydrochloride and 1 5 g. of crystallised sodium acetate in 10 ml. of water if the resulting solution is turbid, filter. Add a solution of 0 5 ml. of cycZohexanone in 8 ml. of water to the reagent... 

Semicarbazones. Dissolve 1 g. of semicarbazide hydrochloride and 1 5g. of crystallised sodium acetate in 8-10 ml. of water add 0 - 5-1 g. of the aldehyde or ketone and shake. If the mixture is turbid, add alcohol (acetone-free) or water until a clear solution is obtained shake the mixture for a few minutes and allow to stand. Usually the semicarbazone crystallises from the cold solution on standing, the time varying from a few minutes to several hours. The reaction may be accelerated,... 

Test the solution so obtained for unsaturation by adding cold 1 per cent, potassium permanganate solution a drop at a time. The immediate disappearance of the purple colour and the formation of a brown turbidity indicates the presence of a double bond Baeyer a test). It must be noted that many substances, not unsaturated, decolourise warm acid or neutral potassium permanganate solution. 

Dissolve or suspend 0 - 5 g. of the acid in 5 ml. of water in a small conical flask, add a drop or two of phenolphthalein indicator, and then 4-5 per cent, sodium hydroxide solution until the acid is just neutrahsed. Add a few drops of very dilute hydrochloric acid so that the final solution is faintly acid (litmus).f Introduce 0-5 g. of p-bromophenacyl bromide (m.p. 109°) dissolved in 5 ml. of rectified (or methylated) spirit, and heat the mixture under reflux for 1 hour if the mixture is not homogeneous at the boiling point or a solid separates out, add just sufficient alcohol to produce homogeneity. [Di- and tri-basic acids require proportionately larger amounts of the reagent and longer refluxing periods.] Allow the solution to cool, filter the separated crystals at the pump, wash with a little alcohol and then with water. Recrystallise from dilute alcohol dissolve the solid in hot alcohol, add hot water until a turbidity just results, clear the latter with a few drops of alcohol, and allow to cool. Acetone may sometimes be employed for recrystallisation. 

The n-capronitrile is sometimes slightly turbid the turbidity is readily removed by shaldng with a little anhydrous calcium sulphate. 

To 5 ml. of water add 1-2 drops of the amine if the amine does not dissolve, add a drop or two of concentrated hydrochloric acid. Add 0-5-1 ml. of this amine solution to 2-3 ml. of the reagent an almost immediate precipitate indicates the presence of a primary amine. A slight turbidity indicates the presence of a primary amine as an impurity. (Primary aromatic amines generally require 2-3 minutes for the test. Urea and other amides, as well as amino acids, do not react.)... 

Introduce 197 g. of anhydrous brucine or 215 g. of the air-dried dihydrate (4) into a warm solution of 139 g. of dZ-acc.-octyl hj drogen phthalate in 300 ml. of acetone and warm the mixture vmder reflux on a water bath until the solution is clear. Upon cooling, the brucine salt (dA, IB) separates as a crystalline solid. Filter this off on a sintered glass funnel, press it well to remove mother liquor, and wash it in the funnel with 125 ml. of acetone. Set the combined filtrate and washings (W) aside. Cover the crystals with acetone and add, slowly and with stirriug, a slight excess (to Congo red) of dilute hydrochloric acid (1 1 by volume about 60 ml.) if the solution becomes turbid before the introduction of... 

The filtrates from the decomposition of the brucine salts with dilute hydrochloride acid should be carefully preserved. The brucine Is recovered by the addition of an excess of dilute ammonia solution (1 4) if the solution becomes turbid before all the ammonia solution is added, introduce a little alcohol until the solution becomes clear. After several hours in an open beaker, filter oft the brucine, wash it well with cold water and dry it in the air. 

To prepare pure anhydrous o-benzoylbenzoic acid, dissolve the air-dried (or the moist) product in about 175 ml. of benzene contained in a 500 ml. round-bottomed flask fitted with a reflux condenser and heat on a water bath. Transfer the benzene solution to a separatory funnel, run oflF any water present, and dry with anhydrous magnesium sulphate. Concentrate the benzene solution to about 75 ml. and add light petroleum, (b.p. 60-80°) to the hot solution until a slight turbidity is produced. Allow to cool spontaneously to room temperature, then cool in ice to about 5°, collect the crystals and dry. The yield of pure, anhydrous o-benzoylbenzoic acid, m.p. 128°, is 32 g. 

The suspension of phenylacetamide may be further hydrolysed to phenylacetic acid by refluxing with stirring until the solid dissolves. The mixture becomes turbid after 30 minutes and the product begins to separate as an oil refluxing is continued for 6 hours, the mixture is cooled first with tap water and then by an ice-water bath for about 4 hours. The crude phenylacetic acid is filtered at the pump, washed with two 50 ml. portions of cold water, and dried in a desiccator. The resulting crude acid melts at 69- 70° it may be purified by recrystallisation from light p>etroleum (b.p. 40-60°) or, better, by vacuum distillation. 

Solubility in 5 per cent, sodium hydroxide solution. Note whether there is any rise in temperature. If the compound appears insoluble, remove some of the supernatant liquid by means of a dropper to a semimicro test-tube (75 X 10 mm.), add 5 per cent, hydrochloric acid dropwise until acid, and note whether any precipitate (or turbidity) is formed. The production of the latter will place the compound in Group III. 

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