Hydrogen from perchloric acid

METHYLCYCLOHEXANONE or o-METHYLCYCLOHEXANONE or 1-METHYL-CYCLOHEXAN-2-ONE (583-60-8) Forms explosive mixture with air (flash point 118°F/48°C cc). Violent reaction with oxidizers, aldehydes, nitric acid, perchloric acid. A variety of unstable peroxides may be formed from the reaction with hydrogen peroxide. Incompatible with aliphatic amines, strong bases, hydrogen peroxide, perchloric acid. Attacks some plastics, rubber, and coatings. 

Positionalisomeri tion occurs most often duting partial hydrogenation of unsaturated fatty acids it also occurs ia strongly basic or acidic solution and by catalysis with metal hydrides or organometaUic carbonyl complexes. Concentrated sulfuric or 70% perchloric acid treatment of oleic acid at 85°C produces y-stearolactone from a series of double-bond isomerizations, hydration, and dehydration steps (57). 

The dimethyl acetal (94) is readily prepared from the 22-aldehyde (93) by direct reaction with methanol in the presence of hydrogen chloride. Ena-mines (95) are formed without a catalyst even with the poorly reactive piperidine and morpholine.Enol acetates (96) are prepared by refluxing with acetic anhydride-sodium acetate or by exchange with isopropenyl acetate in pyridine.Reaction with acetic anhydride catalyzed by boron trifluoride-etherate or perchloric acid gives the aldehyde diacetate. 

Iminium salts are readily available from C protonation of the corresponding enamines (7). Experimentally the procedure is very simple The enamine dissolved in ether or some other solvent is treated with an appropriate acid such as anhydrous hydrogen chloride or 70% perchloric acid. The iminium salt usually separates and is then collected. Protonation at low temperatures... 

The Af-HjO diagrams present the equilibria at various pHs and potentials between the metal, metal ions and solid oxides and hydroxides for systems in which the only reactants are metal, water, and hydrogen and hydroxyl ions a situation that is extremely unlikely to prevail in real solutions that usually contain a variety of electrolytes and non-electrolytes. Thus a solution of pH 1 may be prepared from either hydrochloric, sulphuric, nitric or perchloric acids, and in each case a different anion will be introduced into the solution with the consequent possibility of the formation of species other than those predicted in the Af-HjO system. In general, anions that form soluble complexes will tend to extend the zones of corrosion, whereas anions that form insoluble compounds will tend to extend the zone of passivity. However, provided the relevant thermodynamic data are aveiil-able, the effect of these anions can be incorporated into the diagram, and diagrams of the type Af-HjO-A" are available in Cebelcor reports and in the published literature. 

Glacial acetic acid, pure or mixed with other solvents, is one of the most attractive solvents for the titration of amines. Commercial acetic acid containing not more than 1% of water (Karl Fischer titration check) can be used in normal practice for the highest accuracy, however, the water content must be lowered to about 0.01% by addition of acetic anhydride and standing for 24 h not more than the stoichiometric amount of acetic anhydride should be used in order to avoid possible reactions with active hydrogen-containing analyte components such as primary or secondary amines or alcohols. A similar procedure is followed in the preparation of perchloric acid titrant from the commercial... 

Ethyl sulfate Flammable liquids Fluorine Formamide Freon 113 Glycerol Oxidizing materials, water Ammonium nitrate, chromic acid, the halogens, hydrogen peroxide, nitric acid Isolate from everything only lead and nickel resist prolonged attack Iodine, pyridine, sulfur trioxide Aluminum, barium, lithium, samarium, NaK alloy, titanium Acetic anhydride, hypochlorites, chromium(VI) oxide, perchlorates, alkali peroxides, sodium hydride... 

The determination of neomycin by non-aqueous titration has been described by Penau et all2l. Neomycin base is allowed to react with standardised perchloric acid the excess acid is then back-titrated with potassium hydrogen phtha-late using crystal violet as indicator. To determine the neomycin content of the sulphate salt the same authors precipitated the sulphate with benzidine before reacting the neomycin with perchloric acid. The amount of benzidine required to precipitate the sulphate is calculated from the sulphate content which is itself determined by titration with sodium hydroxide. 

Methylene dichloride [6] and perchloric acid [7] were purified and dosed as described. Silver perchlorate (BDH) was treated in vacuo for a few hours before use. 1-Phenylethyl bromide (Eastman-Kodak) was fractionally distilled under high vacuum and the middle fraction was collected into breakable phials since this compound undergoes a slow decomposition, yielding hydrogen bromide and styrene, when kept in bulk, solutions of it in methylene dichloride were prepared from the original phials by the tipping technique [7]. Styrene was purified [8], dried, and stored [9] as described. Shortly before use it was vacuum-distilled into breakable phials from a microburette. 

The cyclic voltammograms for Pt(llO) and Pt(lOO) in 0.5 M perchloric acid are shown in Fig. 2-26 and Fig. 2—27 respectively. The shapes of the voltammograms for hydrogen adsorption-desorption were significantly different from those in sulfuric add. Although these anion... 

Similar results were obtained for tert-butyl hydroperoxide and perchloric acid in 2-propanol. Thus, it is evident from the decomposition of hydrogen peroxide into free radicals that both heterolytic and homolytic reactions may be catalyzed by hydrogen ions. Further research is needed to investigate proton catalysis in certain homolytic reactions. 

It has been known that the electrolysis in an MeCN- NaClO system generates an acid The hydrogen has to originate from the solvent. A mechanism for hydrogen abstraction from acetonitrile by the electrooxidatively generated radical 104- to produce perchloric acid has been proposed, but no evidence for the succinonitrile formation appeared (Eq. (5)). The detection of the 104- radical by the aid of HSR was tried But it was found to be difficult to differentiate between the perchlorate radical and the radical from chlorine dioxide The electrolysis in a CH Clj—... 

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