Sulphur powder

Rhombic Sulphur. Pour 4-5 ml of chloroform into a dry test tube in a fume cupboard ) and spill in a sulphur powder in small portions, shaking the contents of the tube, until a saturated solution forms. Filter the solution into a porcelain bowl (do not wet the filter with water, why ), cover it with a glass, and let it stand in the fume cupboard for slow evaporation. Put a drop of the solution on a slide, cover it with a cover glass, and observe under a microscope how the crystals grow. Draw the sulphur crystals. 

Plunket s Ointment for Cancer. White arsenic, sulphur, powdered flowers of lesser spearwort and stinking chamomile, levigated together, aud formed mto a paste with white of egg. 

Sulphur, powder Tin, granulated Tin, sheet Zinc, dust Zinc, pure Zinc, sheet Zinc chloride... 

I asked my visitor whether the potion was a preparation of the Philosophers Stone, but he replied that I must not be curious. He added presently that at the bidding of his master he took down a piece of lead water-pipe and melted it in a pot, when the master removed some sulphurous powder on the point of a knife from a little box, cast it into the molten lead, and after exposing the compound for a short time to a fierce fire he poured forth a great mass of liquid gold upon the brick floor of the kitchen. 

Small bags carrying sulphur powder generally have a net content of 50 kg material and a tare weight of 1.0—1.5 kg thus, the total weight of the bags may be 51.0-51.5 kg. 

Sulphur powder can be stored in air open bunkers provided that they have a water-tight roof to keep out the rain. Molten sulphur storage tanks and organic feedstock, sulphonic acid and AD paste tanks can also be located in the open air provided that the local climate is not extremely cold. 

It is prepared by acidifying an alkali solution of anthrone or by reduction of anthraquinone with aluminium powder and concentrated sulphuric acid. 

Crystalline powder, m.p. 174-179 C. Prepared by treatment of thiocarbanilide with sulphur, or by heating aniline, carbon disulphide and nitrobenzene. It is an important rubber accelerator, and on oxidation gives dibenzthiazyl disulphide, also a rubber accelerator. 

Tellurium trioxide, TeOa, is an orange yellow powder made by thermal decomposition of telluric(VI) acid Te(OH)g. It is a strong oxidising agent which will, like H2Se04, oxidise hydrogen chloride to chlorine. It dissolves in hot water to give telluric(VI) acid. This is a weak acid and quite different from sulphuric and selenic acids. Two series of salts are known. 

The crystalline sodium sulphide (NajS,9H20) used to prepare the disulphide is very deliquescent, and only a sample which has been kept in a well-stoppered bottle and therefore reasonably dry should be used. A sample from a badly-stoppered bottle may contain, in addition to the crystals, a certain amount of aqueous solution, in which hydrolysis and partial decomposition will have occurred such a sample should therefore be rejected. Add 4 2 g. of finely powdered sulphur to a solution of 16 g. of the crystalline sodium sulphide in 60 ml. of water, and boil the mixture gently for a few minutes until a clear solution of the disulphide is obtained. 

Dissolve 5 g. (5 ml.) of aniline in 50 ml. of warm dilute sulphuric acid in a conical flask and add 50 ml. of water. Place a thermometer in the solution, immerse the flask in a mixture of ice and water, and cool until the temperature of the stirred solution falls to 5°. Dissolve 4-5 g. of powdered sodium nitrite in 20 ml. of water, and add this solution in small quantities (about 2-3 ml. at a time) to the cold aniline sulphate solution. Keep tne latter well shaken and maintain the temperature at about 5° (see p. 183). When all the sodium nitrite solution has been added, transfer about 5 ml. of the cold solution to a test-tube for each of the following reactions. The remainder of the diazonium hydrogen sulphate solution must be kept in ice-water until required, and then when all the reactions have been carried out, the solution should be poured down the sink. 

Reagent B, Suspend i g. of the powdered dinitrophenylhydrazine in 30 ml. of stirred methanol and cautiously add 2 ml. of concentrated sulphuric acid. If necessary, filter the solution whilst it is still warm and cool the filtrate. 

A 1500 ml. flask is fitted (preferably by means of a three-necked adaptor) with a rubber-sleeved or mercury-sealed stirrer (Fig. 20, p. 39), a reflux water-condenser, and a dropping-funnel cf. Fig. 23(c), p. 45, in which only a two-necked adaptor is shown or Fig. 23(G)). The dried zinc powder (20 g.) is placed in the flask, and a solution of 28 ml. of ethyl bromoacetate and 32 ml. of benzaldehyde in 40 ml. of dry benzene containing 5 ml. of dry ether is placed in the dropping-funnel. Approximately 10 ml. of this solution is run on to the zinc powder, and the mixture allowed to remain unstirred until (usually within a few minutes) a vigorous reaction occurs. (If no reaction occurs, warm the mixture on the water-bath until the reaction starts.) The stirrer is now started, and the rest of the solution allowed to run in drop-wise over a period of about 30 minutes so that the initial reaction is steadily maintained. The flask is then heated on a water-bath for 30 minutes with continuous stirring, and is then cooled in an ice-water bath. The well-stirred product is then hydrolysed by the addition of 120 ml. of 10% sulphuric acid. The mixture is transferred to a separating-funnel, the lower aqueous layer discarded, and the upper benzene layer then... 

Action of sulphuric add. To 0-5 g. of powdered chloral hydrate add 2 ml. of cone. H2SO4, shake well and allow to stand. Liquid chloral gradually separates out as an oil on the surface of the acid. 

Digestion. 20-25 mg. of the substance whose nitrogen content is to be estimated are weighed out in a stoppered weighing-tube and then transferred to the flask L that has been previously dried in an oven at izo C. With care, the substance may be transferred directly into the bulb of the flask without any adhering to the sides. If any material sticks on the way down, the flask should be tapped gently to cause the substance to fall to the bottom. 2 G. of the catalyst mixture (32 g. of potassium sulphate, 5 g. of mercury sulphate and ig. of selenium powder, well mixed) are added and 3 ml. of A.R. cone, sulphuric acid are measured out carefully and poured into the digestion... 

Cuprous bromide. The solid salt may be prepared by dissolving 150 g. of copper sulphate crystals and 87 5 g. of sodium bromide dihydrate in 500 ml. of warm water, and then adding 38 g. of powdered sodium sulphite over a period of 5-10 minutes to the stirred solution. If the blue colour is not completely discharged, a little more sodium sulphite should be added. The mixture is then cooled, the precipitate is collected in a Buchner funnel, washed twice with water containing a little dissolved sulphurous acid, pressed with a glass stopper to remove most of the liquid, and then dried in an evaporating dish or in an air oven at 100 120°. The yield is about 80 g. 

Mix together in a 250 ml. flask carrying a reflux condenser and a calcium chloride drying tube 25 g. (32 ml.) of freshly-distilled acetaldehyde with a solution of 59-5 g. of dry, powdered malonic acid (Section 111,157) in 67 g. (68-5 ml.) of dry pyridine to which 0-5 ml. of piperidine has been added. Leave in an ice chest or refrigerator for 24 hours. Warm the mixture on a steam bath until the evolution of carbon dioxide ceases. Cool in ice, add 60 ml. of 1 1 sulphuric acid (by volume) and leave in the ice bath for 3-4 hours. Collect the crude crotonic acid (ca. 27 g.) which has separated by suction filtration. Extract the mother liquor with three 25 ml. portions of ether, dry the ethereal extract, and evaporate the ether the residual crude acid weighs 6 g. Recrystallise from light petroleum, b.p. 60-80° the yield of erude crotonic acid, m.p. 72°, is 20 g. 

Suspend in a round-bottomed flask 1 g. of the substance in 75-80 ml. of boihng water to which about 0 -5 g. of sodium carbonate crystals have been added, and introduce slowly 4 g. of finely-powdered potassium permanganate. Heat under reflux until the purple colour of the permanganate has disappeared (1-4 hours). Allow the mixture to cool and carefully acidify with dilute sulphuric acid. Heat the mixture under reflux for a further 30 minutes and then cool. Remove any excess of manganese dioxide by the addition of a little sodium bisulphite. Filter the precipitated acid and recrystallise it from a suitable solvent (e.g., benzene, alcohol, dilute alcohol or water). If the acid does not separate from the solution, extract it with ether, benzene or carbon tetrachloride. 

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