Sulphate ferrous

Add about 0 2 g. of ferrous sulphate crystals to the first portion of the filtrate contained in a boiling-tube. An immediate dark greenish-grey precipitate of ferrous hydroxide should occur if the mixture remains clear, add a few ml. of sodium hydroxide solution. Now boil the mixture gently for a few minutes to ensure formation of the ferrocyanide, cool under the tap, add one drop of ferric chloride solution, and then acidify... 

Nitrogen. To one portion of the filtrate, add z-3 ml. of 10, aqueous sodium hydroxide solution, then add about o-2 g. of ferrous sulphate and proceed as in the Lassaigiie nitrogen test (p, 322). Note, however, that the fiUal acidification with dilute siiphiiric acid must be made with care, owing to the vigorous evolution of carbon dioxide from the carbonate present. 

Fenton s reagent. To a solution of tartaric acid or a tartrate add 1 drop of freshly prepared ferrous sulphate solution, i drop of hydrogen peroxide solution and then excess of NaOH solution an intense violet coloration is produced, due to the ferric salt of dihydroxyfumaric acid, HOOC C(OH) C(OH)COOH. 

Ferrous Sulphate. Dissolve 10 g. of FeS04,7H20 in water, add 10 ml. of dil. H2SO4 and make up to 100 ml. with water. It should, whenever possible, be prepared immediately before use. 

Absolute diethyl ether. The chief impurities in commercial ether (sp. gr. 0- 720) are water, ethyl alcohol, and, in samples which have been exposed to the air and light for some time, ethyl peroxide. The presence of peroxides may be detected either by the liberation of iodine (brown colouration or blue colouration with starch solution) when a small sample is shaken with an equal volume of 2 per cent, potassium iodide solution and a few drops of dilute hydrochloric acid, or by carrying out the perchromio acid test of inorganic analysis with potassium dichromate solution acidified with dilute sulphuric acid. The peroxides may be removed by shaking with a concentrated solution of a ferrous salt, say, 6-10 g. of ferrous salt (s 10-20 ml. of the prepared concentrated solution) to 1 litre of ether. The concentrated solution of ferrous salt is prepared either from 60 g. of crystallised ferrous sulphate, 6 ml. of concentrated sulphuric acid and 110 ml. of water or from 100 g. of crystallised ferrous chloride, 42 ml. of concentrated hydiochloric acid and 85 ml. of water. Peroxides may also be removed by shaking with an aqueous solution of sodium sulphite (for the removal with stannous chloride, see Section VI,12). 

CAUTION. Ethers that have been stored for long periods, particularly in partly-filled bottles, frequently contain small quantities of highly explosive peroxides. The presence of peroxides may be detected either by the per-chromic acid test of qualitative inorganic analysis (addition of an acidified solution of potassium dichromate) or by the liberation of iodine from acidified potassium iodide solution (compare Section 11,47,7). The peroxides are nonvolatile and may accumulate in the flask during the distillation of the ether the residue is explosive and may detonate, when distilled, with sufficient violence to shatter the apparatus and cause serious personal injury. If peroxides are found, they must first be removed by treatment with acidified ferrous sulphate solution (Section 11,47,7) or with sodium sulphite solution or with stannous chloride solution (Section VI, 12). The common extraction solvents diethyl ether and di-tso-propyl ether are particularly prone to the formation of peroxides. 

Quinoline may be prepared by heating a mixture of aniline, anhydrous glycerol and concentrated sulphuric acid with an oxidising agent, such as nitrobenzene. The reaction with nitrobenzene alone may proceed with extreme violence, but by the addition of ferrous sulphate, which appears to function as an oxygen carrier, the reaction is extended over a longer period of time and Is under complete control. 

The filtered alkaline solution, resulting from the action of water upon the sodium fusion, is treated with ferrous sulphate and thus forms sodium ferro-eyanide ... 

Nitrogen. Pour 2-3 ml. of the filtered fusion solution into a test-tube containing 0 -1-0-2 g. of powdered ferrous sulphate crystals. Heat... 

If sulphur is present, a black precipitate of ferrous sulphide is obtained when the ferrous sulphate crystals dissolve. Boil the mixture for about 30 seconds, and acidify with dilute sulphuric acid the ferrous sulphide dissolves and a precipitate of Prussian blue forms if nitrogen is present. 

Nitric oxide is made commercially by oxidation of ammonia above 500°C in the presence of platinum, or by reduction of nitrous acid with ferrous sulphate or feiTous halides. The physical ... 

Potassium persulfate with ferrous sulphate was successfully used as the initiator for grafting vinyl monomers onto wool [43] and cellulose [44] by Misra et al. They observed that there exists a critical molar ratio of... 

Besides Fe-, other reducing agents that may be used in conjunction with H2O2 are aliphatic amines, Na2S203 thiourea, ascorbic acid, glyoxal, sulfuric acid, NaHSOs, sodium nitrite, ferric nitrate, peroxidase, AgNOs, tartaric acid, hydroxylamine, ethylene sulfate, sodium phosphite, formic acid, ferrous ammonium sulphate, acetic acid, ferrous sulphate, and HNO2, etc,... 

Critical relative humidity The primary value of the critical relative humidity denotes that humidity below which no corrosion of the metal in question takes place. However, it is important to know whether this refers to a clean metal surface or one covered with corrosion products. In the latter case a secondary critical humidity is usually found at which the rate of corrosion increases markedly. This is attributed to the hygroscopic nature of the corrosion product (see later). In the case of iron and steel it appears that there may even be a tertiary critical humidity . Thus at about 60% r.h. rusting commences at a very slow rate (primary value) at 75-80% r.h. there is a sharp increase in corrosion rate probably attributable to capillary condensation of moisture within the rust . At 90% r.h. there is a further increase in rusting rate corresponding to the vapour pressure of saturated ferrous sulphate solution , ferrous sulphate being identifiable in rust as crystalline agglomerates. The primary critical r.h. for uncorroded metal surfaces seems to be virtually the same for all metals, but the secondary values vary quite widely. 

Thus for non-ferrous metals, SO is consumed in the corrosion reactions whereas in the rusting of iron and steel it is believed that ferrous sulphate is hydrolysed to form oxides and that the sulphuric acid is regenerated. Sulphur dioxide thus acts as a catalyst such that one SOj" ion can catalyse the dissolution of more than 100 atoms of iron before it is removed by leaching, spalling of rust or the formation of basic sulphate. These reactions can be summarised as follows ... 

Weather conditions at the time of initial exposure of zinc and steel have a large influence on the protective nature of the initial corrosion products This can still be detected some months after initial exposure. Finally, rust on steel contains a proportion of ferrous sulphate which increases with increase in SO2 pollution of the atmosphere. The effect of this on corrosion rate is so strong that mild steel transferred from an industrial atmosphere to a rural one corrodes for some months as though it was still exposed to the industrial environment. ... 

Sulphur dioxide in the air originates from the combustion of fuel and influences rusting in a number of ways. For example, Russian workers consider that it acts as a cathodic depolariser , which is far more effective than dissolved oxygen in stimulating the corrosion rate. However, it is the series of anodic reactions culminating in the formation of ferrous sulphate that are generally considered to be of particular importance. Sulphur dioxide in the air is oxidised to sulphur trioxide, which reacts with moisture to form sulphuric acid, and this in turn reacts with the steel to form ferrous sulphate. Examination of rust Aims formed in industrial atmospheres have shown that 5% or more of the rust is present in the form of iron sulphates and FeS04 4H2 0 has been identified in shallow pits . 

Temperature is the most important of the factors affecting pickle activity. In general, an increase of 10°C causes an increase in pickling speed of about 70 Vo. Agitation of the pickle increases the speed since it assists the removal of the insoluble scale and rapidly renews the acid at the scale surface. Increase in acid concentration up to about 40 Vo w/w in ferrous sulphate-free solutions, and up to lower concentrations in solutions containing ferrous sulphate, increases the activity. Increase in the ferrous sulphate content at low acid concentrations reduces the activity, but at 90-95 C and at acid concentrations of about 30 Vo w/w it has no effect. 

For the batch pickling of rod, sheet, tube or strip in coil form, short pickling times are not so important, and pickling times of several minutes at 60-80°C in 5-10% w/w acid are common. The acidity is maintained by the addition of fresh strong acid, until the pickle is nearly saturated with ferrous sulphate, and then the acidity is worked down to 1 or 2%. 

Atmospheric exposure trials, carried out in Cambridge, established the fact that when rusty specimens were painted in the summer, their condition, after some years exposure, was very much better than that of similar specimens painted in the winter It was found that steel weathered in Cambridge carried spots of ferrous sulphate, deeply imbedded in the rust, and that the quantity of ferrous sulphate/unit area was very much greater in the winter than in the summer this seasonal variation was attributed to the increased sulphur dioxide pollution of the atmosphere in the winter, caused by the combustion of coal in open grates. It was concluded that there was a causal relationship between the quantity of ferrous sulphate and the effective life of the paint. It was suggested that these soluble deposits of ferrous sulphate short-circuit the resistance of the paint film and, since paint films are very permeable to water and oxygen, the ferrous sulphate will become oxidised and hydrolysed with the production of voluminous rust, which will rupture the film at numerous points, thus giving rise to the characteristic type of failure seen on painted rusty surfaces. 

It can be claimed that the problem of painting rusty surfaces is now understood. A method for estimating the ferrous sulphate content of any rusty surface has been put forward, but the amount of ferrous sulphate... 

The inspector s working standard for the surface finish of blast-cleaned steel is now the new British Standard . In the special circumstances where absolute freedom from soluble contaminants such as ferrous sulphate is necessary, the specification should include reference to a test for removal of such residual salts, e.g. the potassium ferricyanide test . The area to be sampled should be wetted with a fine spray of distilled water and the paper held against it. The development of blue spots on the paper indicates the presence of ferrous salts on the surface. 

Ferrous ammonium sulphate Ferrous chloride Ferrous sulphate Lead nitrate Lithium chloride... 

Bismuth sulphite agar. This medium was developed in the 1920s for the identification of Salmonella typhi in water, faeces, urine, foods and pharmaceutical products. It consists of a buffered nutrient agar containing bismuth sulphite, ferrous sulphate and brilliant green. 

Both of these rate laws combine in that for the autoxidation of ferrous sulphate at 140-180 C° in dilute sulphuric acid solution viz. 

A veterinary preparation made with diarsenic trioxide, sodium nitrate and ferrous sulphate combusted spontaneously. 

Picoline reacted very violently and suddenly with 30% hydrogen peroxide when ferrous sulphate was present. The apparatus detonated and the gases and liquids that spread caused a violent fire. The accident was put down to the fact that the medium was not stirred enough. 

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