Hydrogen sulphide preparation

CfiHsNjOs. Red needles m.p. 168-169°C. Soluble in dilute acids and alkalis. Prepared by reduction of picric acid with sodium hydrogen sulphide, ft is used for the preparation of azodyes, which can be after-chromed by treatment with metallic salts owing to the presence of a hydroxyl group ortho to the amino-group. 

To prepare gas for evacuation it is necessary to separate the gas and liquid phases and extract or inhibit any components in the gas which are likely to cause pipeline corrosion or blockage. Components which can cause difficulties are water vapour (corrosion, hydrates), heavy hydrocarbons (2-phase flow or wax deposition in pipelines), and contaminants such as carbon dioxide (corrosion) and hydrogen sulphide (corrosion, toxicity). In the case of associated gas, if there is no gas market, gas may have to be flared or re-injected. If significant volumes of associated gas are available it may be worthwhile to extract natural gas liquids (NGLs) before flaring or reinjection. Gas may also have to be treated for gas lifting or for use as a fuel. 

Sulphur can be reduced directly to hydrogen sulphide by passing hydrogen through molten sulphur the reversible reaction H2 -I-S H2S occurs. In the laboratory the gas is most conveniently prepared by the action of an acid on a metal sulphide, iron(II) and dilute hydrochloric acid commonly being used ... 

These two gases can readily be prepared by the action of acids on selenides and tellurides respectively, the reactions being analogous to that for the preparation of hydrogen sulphide. 

These are ionic solids and can exist as the anhydrous salts (prepared by heating together sulphur with excess of the alkali metal) or as hydrates, for example Na2S.9HjO. Since hydrogen sulphide is a weak acid these salts are hydrolysed in water,... 

They are rapidly hydrolysed by water and the hydrolysis of solid aluminium sulphide can be used to prepare hydrogen sulphide ... 

These are practically insoluble in water, are not hydrolysed and so may be prepared by addition of a sufficient concentration of sulphide ion to exceed the solubility product of the particular sulphide. Some sulphides, for example those of lead(II), copper(II) and silver(I), have low solubility products and are precipitated by the small concentration of sulphide ions produced by passing hydrogen sulphide through an acid solution of the metal salts others for example those of zincfll), iron(II), nickel(II) and cobalt(II) are only precipitated when sulphide ions are available in reasonable concentrations, as they are when hydrogen sulphide is passed into an alkaline solution. 

An aqueous solution of hydrogen iodide, up to 50% strength, may be prepared by passing hydrogen sulphide (or sulphur dioxide) into a suspension of iodine in water ... 

Lead formate separates from aqueous solution without water of crystallisation. It can therefore be used for the preparation of anhydrous formic acid. For this purpose, the powdered lead formate is placed in the inner tube of an ordinary jacketed cond ser, and there held loosely in position by plugs of glass-wool. The condenser is then clamped in an oblique position and the lower end fitted into a receiver closed with a calcium chloride tube. A current of dry hydrogen sulphide is passed down the inner tube of the condenser, whilst steam is passed through the jacket. The formic acid which is liberated... 

Hydrogen sulphide. This poisonous gas is usually prepared from ferrous sulphide and dilute hydiochloric acid (1 3) in a Kipp s apparatus it should be washed with water to remove acid spray. 

In a 1 litre round-bottomed flask provided with an efficient double surface condenser, place 40 g. (39 ml.) of aniline, 50 g. (40 ml.) of carbon sulphide CAUTION inflammable) (1), and 50 g. (63-5 ml.) of absolute ethyl alcohol (2). Set up the apparatus in the fume cupboard or attach an absorption device to the top of the condenser (see Fig. 11, 8, 1) to absorb the hydrogen sulphide which is evolved. Heat upon an electrically-heated water bath or upon a steam bath for 8 hours or until the contents of the flask sohdify. When the reaction is complete, arrange the condenser for downward distillation (Fig. 11, 13, 3), and remove the excess of carbon disulphide and alcohol (CA UTION inflammable there must be no flame near the receiver). Shake the residue in the flask with excess of dilute hydrochloric acid (1 10) to remove any aniline present, filter at the pump, wash with water, and drain well. Dry in the steam oven. The yield of crude product, which is quite satisfactory for the preparation of phenyl iao-thiocyanute (Section IV.95), is 40-45 g. Recrystalhse the crude thiocarbanihde by dissolving it, under reflux, in boiling rectified spirit (filter through a hot water funnel if the solution is not clear), and add hot water until the solution just becomes cloudy and allow to cool. Pure sj/m.-diphenylthiourea separates in colourless needles, m.p, 154°,... 

The acid is conveniently prepared by the reduction of p-nitrophenylacetic acid with ammonium sulphide (hydrogen sulphide in ammoniacal solution). 

Sulphur. Moisten the centre of a filter paper with sodium plumbite solution. Add about 10 ml. of dilute hydrochloric acid to the residue in the dish and immediately cover it with the prepared filter paper. If zinc sulphide is present in the residue, a dark brown stain, visible on the upper surface of the paper, will be obtained frequently the presence of hydrogen sulphide can also be detected by its odour. 

Hydrogen sulphide is usually prepared on a small seale by the aetion of hydroehlorie aeid on ferrous sulphide ... 

Hydrogen sulphide is used in the preparation of metal sulphides, oil additives ete., in the purifieation and separation of metals, as an analytieal reagent and as raw material in organie synthesis. It burns in air with a blue flame ... 

Procedure To each of the cylinders containing the standard solution and test solution respectively, add 10 ml of freshly prepared hydrogen sulphide solution, mix, dilute with water (DW) to 50 ml, allow to stand for 5 minutes and view downwards over a white surface, the colour produced in the test solution is not darker than that produced in the standard solution. 

Hydroxy-4-methylthiazole-2(3//)thione carbamates, e.g. the cyclohexyl derivative 336, are precursors for monoalkylaminium cation radicals, which cannot be prepared from 2-thioxopyridinyloxycarbamates. The carbamate is obtained from 3-hydroxy-4-methylthiazole-2(3//)-thione and cyclohexyl isocyanate. When irradiated in the presence of malonic acid and /-butyl hydrogen sulphide it yields the cyclohexylaminium cation... 

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