Iron, Electrolytic

The original German process used either carbonyl iron or electrolytic iron as hydrogenation catalyst (113). The fixed-bed reactor was maintained at 50—100°C and 20.26 MPa (200 atm) of hydrogen pressure, giving a product containing substantial amounts of both butynediol and butanediol. Newer, more selective processes use more active catalysts at lower pressures. In particular, supported palladium, alone (49) or with promoters (114,115), has been found useful. 

Smooth oxidized electrolytic iron 260-980 0.78-0.82 Oxidized by heating at 750 F. 750 0.11... 

Potassium permanganate can be standardized by titration of sodium oxalate (Na2C204) by Reaction 7-1 or pure electrolytic iron wire. Dissolve dry (105°C, 2 h) sodium oxalate (available in a 99.9-99.95% pure form) in 1 M H2S04 and treat it with 90-95% of the required KMn04 solution at room temperature. Then warm the solution to 55-60°C and complete the titration by slow addition of KMn04. Subtract a blank value to account for the quantity of titrant (usually one drop) needed to impart a pink color to the solution. 

Ingredient Ingot iron Electrolytic iron Carbonyl iron Hydrogen-puri fied iron... 

Treatment of Graphite to Increase Iron. Iron in some form is known to be present in Aquadag and in many other sources of graphite. A graphite of low iron content, Air-Spun Type 200-10, was treated to increase its iron content by intimate mixing with electrolytic iron dust. The mixture was heated overnight in a 400° C. furnace, and then treated with mixed acid. An electrode prepared from this product, dispersed with tannic acid, was compared with an electrode made from mixed acid-treated, tannic acid-dispersed stock Air-Spun. 

An alternate synthesis of 3,4-methylenedioxyphenylacetone starts originally from piperonal. A suspension of 32 g electrolytic iron in 140 mL glacial acetic acid was gradually warmed on the steam bath. When quite hot but not yet with any white salts apparent, there was added, a bit at a time, a solution of 10.0 g of l-(3,4-methylenedioxyphenyl)-2-nitropropene in 75 mL acetic acid (see the synthesis of MDA for the preparation of this nitrostyrene intermediate from piperonal and nitroethane). This addition was conducted at a rate that permitted a vigorous reaction free from excessive frothing. The orange color of the reaction mixture... 

A solution of 4.0 g of l-(3,4-ethylenedioxyphenyl)-2-nitropropene was made in 30 mL warm acetic acid. This was added to a suspension of 16 g elemental electrolytic iron in 75 mL acetic %cid. The mixture was heated on the steam bath, and an exothermic reaction set in at about 70 °C. Heating was continued and the... 

G. J. Fowler by heating ferrous chloride or bromide in ammonia. H. Hanemann used electrolytic iron foil A. H. White... 

Ferrous chloride from commercial sources may contain ferric chloride and is likely to be too acid. If this is allowed to stand in contact with excess iron, preferably powder, a satisfactory solution becomes available. If very pure derivatives are desired, the ferrous chloride may be prepared directly from pure hydrochloric acid and electrolytic iron. 

Figure 3b. Morphology plot for adipic acid ATM — atomized iron, RED - reduced iron, ELECT — electrolytic iron. Reproduced with permission from Ref. 2. Copyright 1984 CRC Press.

A suspension of 1.7 g electrolytic iron dust in 10 mL of 80% aqueous acetic acid was heated on the steam bath until there were clear signs of hydrogen evolution. 

When electrolytic iron foil is heated in steam to about 330° C., tarnishing begins to take place. At 400° C. a small but measurable quantity of hydrogen is formed, and the velocity of the reaction increases rapidly with further rise of temperature The reaction appears to take place m three stages, involving2... 

According to Noyes, the minimum potential required for the electrolysis of an aqueous solution of a ferrous salt at 20° C. is 0-66 volt, when electrodes of electrolytic iron are employed.3 This value falls by 0-007 volt per degree rise in temperature up to 110° C., when it attains a minimum. Further rise in temperature necessitates an increased voltage. 

Electrolytic iron deposited from solution at ordinary pressures and temperatures is apt to be admixed with ferric hydroxide, and to contain hydrogen6 and carbon. The last-named element is commonly derived from the oxalates or tartrates m the baths, when these are used, and as the result of transfer from the anodes. The carbon may be free, combined as carbide, or present as occluded carbon monoxide or dioxide. 

Electrolytic iron is frequently brittle, a property that is usually attributed to occluded hydrogen,7 but there are probably other auxiliary causes.8... 

When electrolytic iron foil is immersed in concentrated solutions of jodium or potassium hydroxide for several weeks, and, after thorough cleaning, allowed to corrode in distilled water, the latter gradually becomes contaminated with traces of sodium or potassium salts, the bresence of which can be detected by the spectroscope or by the usual Bunsen flame test.6 Similar results have been obtained with lithium lydroxide, barium hydroxide, and with ammonia.7 It appears probable hat the alkali penetrates in minute quantities into the metal between he ferrite crystals, possibly in consequence of a certain amount of borosity in the intercrystalline cement. This theory is supported by he fact that iron which has been soaked in alkali invariably pits ... 

Drainage water from coal mines is frequently charged with ferrous sulphate consequent upon the oxidation of pyrites in the coal, and upon evaporation yields the impure salt. The salt is readily obtained in a pure state by dissolving electrolytic iron in dilute sulphuric acid and allowing to crystallise, preferably in an inert atmosphere. Commercially ferrous sulphate is obtained by exposing heaps of pyrites to the oxidising action of the air. Ferrous sulphate and free sulphuric acid drain off into tanks, the acid being neutralised with scrap iron —... 

SYNS ANCOR EN 80/150 ARMCO IRON CARBONYL IRON EFV 250/400 EO 5A FERROVAC E GS 6 IRON, CARBONYL (FCC) IRON, ELECTROLYTIC IRON, ELEMENTAL ... 

Other primary standards are pure electrolytic iron Fe(II) ammonium sulfate, FeS04-(NH4)2S04-6H20 potassium ferrocyanide, K4[Fe(CN)g] 3H20 and potassium iodide. Permanganate often is used without an indicator since a 2 x 10" M solution has a discernible pink color. 

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