Purification of Solvents for Electroanalysis: Tetrahydrofuran and Dioxane
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Abstract:
This report is a continuation of the same project of the Commission on Electroanalytical Chemistry which led to the publication in 1982 of the compilation Recommended Methods for Purification of Solvents and Tests for Impurities (Pergamon Press) in which ten protic and aprotic solvents are discussed. The present report is the first to deal with the important class of saturated cyclic ethers, solvents that are used extensively in organometallic chemistry and battery technology. Key properties and uses of these solvents are briefly outlined. In the discussion of recommended purification methods and tests for impurities special emphasis is placed on the presence of peroxides which constitutes a serious explosion hazard in the handling of many ethers.Keywords:
Tetrahydrofuran
Chlorinated solvents
The crystal structure of the complex μ-chloro-μ-hydroxo-bis[dichlorobis(tetrahydrofuran-O)vanadium(III)] tetrahydrofuran solvate, [V2(μ-Cl)(μ-OH)Cl4(thf)4].thf (where thf is tetrahydrofuran, C4H8O), was determined. It was obtained from a tetrahydrofuran solution containing [VCl3(thf)3] and NaCPh3. The two octahedral vanadium(III) centers are bridged by a Cl− and an OH− anion, with a V⋯V separation of 3.281 (1) Å. One vanadium(III) center has two axial Cl and two equatorial tetrahydrofuran ligands, while the other vanadium(III) center has two axial tetrahydrofuran and two equatorial Cl ligands. A tetrahydrofuran molecule which is contained as crystalline solvent is involved in hydrogen bonding with the bridging OH− anion.
Tetrahydrofuran
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This chapter contains sections titled: Properties of Solvents Physical Properties of Solvents Chemical Properties of Solvents Structural Aspects of Solvents Toxicity and Hazardous Properties of Solvents Classification of Solvents Effects of Solvent Properties on Chemical Reactions (an Outline)
Chlorinated solvents
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Tetrahydrofuran
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Reaction of carbazole with barium metal in dry tetrahydrofuran yields colourless blocks of the title compound, [Ba(C4H8O)5](C12H8N)2.C4H8O. The structure contains sevenfold-coordinated barium counter cations, which are surrounded by two carbazole monoanions and five tetrahydrofuran molecules in a C2 symmetric environment.
Tetrahydrofuran
Barium
Carbazole
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Tetrahydrofuran
Isothermal process
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Tetrahydrofuran
Bar (unit)
Clathrate hydrate
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Abstract Reduction of relatively conformationally rigid cyclic ketones with sodium borohydride was examined in a mixed solvent of tetrahydrofuran(THF) and methanol(MeOH) with varying the ratio of the components. The highest stereoselectivities of the reductions were observed in the mixed solvent, and not in each individual solvent.
Tetrahydrofuran
Sodium borohydride
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Chlorinated solvents
Environmental Analysis
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Phase equilibria (pressure−temperature relations) of the H2 + tetrahydrofuran mixed gas hydrate system have been measured for various concentrations of tetrahydrofuran aqueous solutions. The three-phase equilibrium lines obtained in the present study are shifted to the low-temperature or high-pressure side from that of the stoichiometric THF solution. Each three-phase equilibrium line of H2 + tetrahydrofuran hydrate converges at the three-phase equilibrium line of the pure tetrahydrofuran hydrate. At the cross point on the lines, the tetrahydrofuran concentration of mother aqueous solution agrees with each other. The Raman spectra of H2 and tetrahydrofuran for the H2 + tetrahydrofuran mixed gas hydrate do not change with the variation of tetrahydrofuran mole fraction from 0.010 to 0.130 in the aqueous solution.
Tetrahydrofuran
Clathrate hydrate
Mole fraction
Stoichiometry
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