Donald E. Sands

Rare-earth trishexafluoroacetylacetonates and related compounds☆

Abstract Rare-earth trishexafluoroacetylacetonates, Ln(hfac)3·nH2O, have been prepared and characterized by chemical analyses, infra-red spectra, and X-ray powder diffraction patterns. Two series of hydrates exist: Ln(hfac)3·3H2O (Ln = LaNd) and Ln(hfac)3·2H2O (Ln = LaLu). No evidence for a lower hydrate was found. A mixed ligand chelate, Ln(hfac)2CF3CO2·2H2O, is a byproduct of the tris chelate preparations. Several series of salts were also prepared, including NH4Ln (hfac)4·nH2O (n = 0 and 1 for Ln = LaNd; n = 0 for Ln = SmLu), pyHLn(hfac)4·nH2O (n = 0 and 1 for Ln = LnNd; n = 0 for Ln = SmLu), and (pyH)2Ln(hfac)5 (Ln = LaNd). Ln(hfac)3·3H2O. NH4Ln(hfac)4·H2O, and pyHLn(hfac)4·H2O are reversibly converted with great ease to Ln(hfac)3·2H2O, NH4Ln(hfac)4, and pyHLn(hfac)4, respectively. Most of the chelates studied are probably eight-co-ordinate, including Ln(hfac)3·3H2O, NH4Ln(hfac)4·H2O, and pyHLn(hfac)4·H2O, but (pyH)2Ln(hfac)5 may be ten-co-ordinate.

Spectra and Structure of Crystalline Cyclopropane and Cyclopropane‐D6

Infrared and Raman spectra of polycrystalline C3H6 and C3D6 were measured between 10 and 3500 cm−1 at 85°K. Infrared spectra of mixed C3H6 and C3D6 crystals were also obtained. From these measurements, an assignment of the origin of the multiplet splittings is proposed. An x‐ray diffraction study of crystalline C3H6 suggests an orthorhombic unit cell with a = 10.0 A, b = 6.8 A, and c = 5.1 A. Density measurements, spectroscopic data, and diffraction data indicate that the site group is Cs and that the space group is one of eight primitive D2h groups. Far‐infrared spectra of crystalline C3H6 showed five absorptions attributed to k = 0 external modes.

ACETYLACETONE ADDUCTS OF RARE EARTH TRIS-THENOYLTRIFLUOROACETONATES IN SYNERGISTIC SOLVENT EXTRACTION.

The synergistic effect of acetylacetone (Hacac) in the extraction of rare earth thenoyltrifluoroacetonates (Mtta3) was attributed to the formation of the species Mtta3 · Hacac. The adduct was isolated and identified by chemical analyses and i.r. spectra.

Boron Modifications Produced in an Induction-Coupled Argon Plasma

Most of the small particles (50 to 100 micrometers in diameter) of microcrystalline β-rhombohedral boron that quickly transit an argon plasma maintained within a radio-frequency induction-coupled torch emerge as better crystallized spheroids of the same crystalline form and nearly the same size as the starting material. A few crystals of each of four distinctive, well-faceted habits are formed along with the general product. Three of these types are monocrystals of the β-rhombohedral polymorph, of the tetragonal-III modification, and of an unreported cubic form of boron. Specimens of the fourth type are polycrystals of another unreported form of boron, apparently consisting of many hexagonal platelets stacked in an imprecise fashion.

Some adducts of rare earth acetylacetonates

Abstract Several previously unreported adducts of rare earth acetylacetonates have been prepared and characterized by chemical analyses (including Karl Fischer titrations for water), i.r. spectra, and X-ray powder diffraction patterns. These adducts include compounds with methanol, ethanol, propanol, butanol, dioxane, pyridine, 2- and 4- methylpyridine, 2,4- and 2,6-dimethylpyridine, acetone, benzene, and acetylacetoneimine. Most of the adducts contain one or more moles of water per mole of chelate. It is concluded that when water and an organic donor are both present, only the water is coordinated to the rare earth ion and that the organic donor molecules are hydrogen-bonded or held in the crystal by lattice forces.

Synergistic solvent extraction of rare earths by mixtures of thenoyltrifluoroacetone and acetylacetone

Abstract The synergistic extraction of the thenoyltrifluoroacetonates of neodymium, samarium, gadolinium, dysprosium, and erbium by acetylacetone was studied using mixtures of the two β-diketones. The synergistic shift of the extraction curves decreases the separability of the rare earth chelates.

Biological techniques in electron microscopy: By Clinton J. Dawes. Barnes and Noble, New York, 1971. xiv + 193 pp. Paperback,

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