Silver mercuri-iodide preparation

Standard methods which convert alkylmercury iodides into bis(alkyl)-mercurials fail to convert perfluoroalkylmercury iodides into bis(perfluoro-alkyl)mercurials. The preparation of primary bis(perfluoroalkyl)mercurials can be accomplished by treating perfluoroalkylmercury iodides with silver, copper, or cadmium amalgams. Alternatively, the parent perfluoroalkyl iodide will react directly with the amalgam. By either method yields are from 40 to 90%. 

Titanium diiodide may be prepared by direct combination of the elements, the reaction mixture being heated to 440°C to remove the tri- and tetraiodides (145). It can also be made by either reaction of soHd potassium iodide with titanium tetrachloride or reduction of Til with silver or mercury. 

Complex [(CXI )Ir(/j,-pz)(/i,-SBu )(/j,-Ph2PCH2PPh2)Ir(CO)] reacts with iodine to form 202 (X = I) as the typical iridium(II)-iridium(II) symmetrical species [90ICA(178)179]. The terminal iodide ligands can be readily displaced in reactions with silversalts. Thus, 202 (X = I), upon reaction with silver nitrate, produces 202 (X = ONO2). Complex [(OC)Ir(/i,-pz )(/z-SBu )(/i-Ph2PCH2PPh2)Ir(CO)] reacts with mercury dichloride to form 203, traditionally interpreted as the product of oxidative addition to one iridium atom and simultaneous Lewis acid-base interaction with the other. The rhodium /i-pyrazolato derivative is prepared in a similar way. Unexpectedly, the iridium /z-pyrazolato analog in similar conditions produces mercury(I) chloride and forms the dinuclear complex 204. 

Tri-p-tolyl tellurium iodide1 melts with decomposition at 232° to 233° C., dissolves readily in methyl alcohol or chloroform, less readily in benzene or ether, and is insoluble in water. Tri-p-tolyl tellurium bromide occurs when the iodide or chloride is boiled with silver bromide. It melts at 265° to 266° C. with decomposition, and dissolves in alcohols or chloroform, but is insoluble in benzene or ether. Tri-p-tolyl tellurium chloride is prepared from the bromide in the usual way. It melts at 260° to 261° C. and gives precipitates with the chlorides of mercury, tin and gold, picric acid and platinic chloride. The hydroxide is a resin, melting at about 110° C., and yielding a pier ate, consisting of long prisms, M.pt. 194° to 195° C.a... 

Establishing the surface area is the next concern. Electrode surfaces are seldom flat. Instead, they tend to display a set of different crystal faces. Sliver Iodide electrodes, prepared by amalgamation of silver with mercury, followed by vapour deposition of iodine, look smooth and shiny to the naked eye but reveeil crystallites under the electron microscope. Surface Irregularities not only complicate the assessment of the real area, they may also Interfere in the analysis of impedance spectra In terms of equivalent circuits. After drying, the surface may be studied by the usual optical methods (sec. 1.2) with the famlllrir caveat that drying may change these properties. Anyway, for a number of oxides and silver iodide It Is now established that electrodes can be made which have... 

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