Sodium—continued sulphide

A quantitative yield of sodium monosulphide is obtained by heating sodium hydrogen sulphide very gradually, the evolved hydrogen sulphide being continually removed 10... 

Mix intimately in a mortar 100 g. of sodium laevulinate, 250 g. of phosphorus sulphide (1) and 50 g. of clean dry sand. Place the mixture in a flask fitted with a condenser for distillation and a receiver (2). Heat the flask with a free flame until the reaction commences, and then remove the flame. When the reaction subsides, continue the heating until distillation ceases. Wash the distillate with 10 per cent, sodium hydroxide solution to remove acidic by-products and steam distil. Separate the crude 2-methyltliiophene from the steam distillate, dry over anhydrous calcium sulphate, and distil from a little sodium. Collect the pure compound at 113° the yield is 30 g. 

The trend in architectural applications has been towards more matt finishes, and the sodium hydroxide-based etchants used frequently contain additives such as sodium nitrate or nitrite or sodium fluoride. Chelating agents such as gluconates, heptonates or sorbitol are added to complex the aluminium produced, and other additives such as sulphides may be present in the etchant to complex zinc dissolved from the alloy, and allow it to be used continuously without dumping ... 

Two grams of sodium were dissolved in absolute alcohol, freshly distilled over quicklime, in a flask fitted with a reflux condenser. As sodium ethoxide began to separate out, more alcohol was added until just sufficient was present to retain the product in soln. at the room temp.—40 c.o. were needed. The flask was fitted with a 2-hole stopper fitted with delivery and egress tube to which calcium chloride tubes were attached. Hydrogen sulphide washed in water, and dried by a long column of calcium chloride was passed rapidly into the soln. A fine crystalline precipitate formed in the soln., and increased in amount with the continued passage of the gas. When the soln. was sat. with gas, the precipitate was collected, rapidly filtered, washed with absolute alcohol, and dried in vacuo over calcium chloride. The precipitate weighed 0 25 grm. When benzene or ether is added to the soln., a precipitate of pure anhydrous sodium hydrosulphide is obtained. This is washed and dried as before. 

J. A. C. Gren observed that an aq. soln. of sodium sulphide is decomposed by carbon dioxide forming sodium carbonate with the evolution of hydrogen sulphide and if the stream of carbon dioxide be continued, sodium bicarbonate is formed. Over fifty patents based upon these observations were obtained. E. Berl and A. Rittener have studied the action of carbon dioxide upon sodium and calcium sulphides. The reaction is by no means simple, for a great proportion of the sodium is converted into bicarbonate before the whole of the sodium sulphide has been decomposed indeed, hydrogen sulphide still escapes even in the advanced stage of the process, where the sodium is almost entirely present as bicarbonate, and the... 

Preparation of Antimony. Put a thoroughly dried mixture of 12 g of antimony sulphide, 5 g of reduced powdered iron, 1.5 g of sodium sulphide, and 0.5 g of powdered charcoal into a chamotte or porcelain crucible and roast it in a muffle furnace at 800 °C. After the entire mixture softens, continue the heating for another 20-30 minutes. Next cool the crucible, break it, and extract the antimony bead. 

Tho inventor prefers to apply this mode of concentration for obtaining soda from vat liquors, to such liquors as have been already deprived of a considerable portion of die carbonate of soda previously contained therein,. Tho circulation of these liquors through the tower Is continued until it ts found that tho whole, or nearly the whole, of the carbonate of soda is removed, when the liquor is separated from the deposited salts, and by further evaporation in an iron pan solid hydrate of soda is obtained, Tho separatod Saits, after being washed, are transferred to a reverberatory furnace and completely dried. The product of those Operations, whichever of the foregoing be adopted, is the white ash or soda ash of commerce. When properly prepared it contains fifty-three or fifty-four per cent, of available soda, two or three of which exist in the form of hydrate,-and the rest as carbonate of soda, A little sulphide of sodium is also present, and some Sulphate of soda, chloride of sodium, and minute quantities of other salts,. 

Stir 2.35 g (0.011 mol) of sodium metaperiodate (Section 4.2.55, p. 454) in 45 ml of a 1 1 mixture of water and methanol held at 0°C. Add portionwise 2.14 g (0.01 mol) of dibenzyl sulphide (Expt 5.204) and continue to stir the mixture at 0 °C for several hours, preferably overnight. Extract the reaction mixture (which contains precipitated sodium iodate) with three 20 ml portions of chloroform. Dry the combined chloroform extracts over magnesium sulphate and remove the solvent on a rotary evaporator. Recrystallise the product from ethanol. The yield of dibenzyl sulphoxide is 2.2 g (96%), m.p. 135 °C. 

The sodium salt,1 NaFe(N0)2S203.2H20, is obtained in a similar manner to the preceding salt. It yields either laminated or needle-shaped crystals, which are glistening black in appearance. They are appreciably more soluble in water than those of the potassium salt, and yield a deep brown solution. The salt is fairly stable below 0° C., but above that temperature continuously evolves nitric oxide. When its aqueous solution is boiled, sulphur dioxide is expelled and ferric hydroxide precipitated. Upon concentrating the clear solution obtained by filtering, crystals of sodium ferro-heptanitroso sulphide, NaFe4(N0)7S3.H20, separate out.2... 

When azo benzene is reduced or when the reduction of nitro benzene is continued beyond the stage of the azo compound we obtain hydrazo benzene, a colorless crystalline solid, m.p. 126°. The reduction may be accomplished (i) by using zinc and alcoholic sodium hydroxide, (2) by means of an alcoholic solution of ammonium sulphide or (3) electro-lytically in the presence of an alkali. 

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