Direct observation of alkyl/nitrosyl migratory insertion in an organotransition metal complex

Treatment of [PdCl2(cod)] with tetrabenzyltin gives the benzylpalladium complex [PdCl(CH2Ph)(cod)] (cod = 1,5-cyclooctadiene), 1a, whose structure has been determined by X-ray crystallography. It adopts approximate square-planar geometry, with the double bonds perpendicular to the square plane. The corresponding ethylpalladium derivative 1b has been prepared by a similar method, but it is considerably less stable. It decomposes by (β-elimination to produce ethene and a transient hydride complex, which either undergoes migratory insertion to give [Pd2(μ-Cl)2(η1,η2-C8H13)2], 2a, or dinuclear reductive elimination with a second molecule of 1b to produce ethane, [PdCl2(cod)], free cyclooctadiene, and palladium metal. Complex 2a has also been prepared by reaction of [PdCl2(cod)] with NaBH4. At higher temperatures 2a converts to an equilibrium mixture with its η3-allyl isomer, 2b. Reactions of [PdCl2(cod)] or K2PdCl4 in the presence of cyclooctadiene in aqueous solution to produce 2a or 2b have also been investigated. Key words: palladium, diene complexes, allyl complexes, isomerization, β-elimination.

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Direct Observation of Heat Exchanger Deposits by Cross Sectioning

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100061835 ◽

1967 ◽

Vol 25 ◽

pp. 364-365

Author(s):

R. W. Anderson ◽

D. L. Senecal

Keyword(s):

Electron Microscopy ◽

Transmission Electron Microscopy ◽

Heat Exchanger ◽

Direct Observation ◽

Cross Sections ◽

Preparation Method ◽

Specimen Preparation ◽

Flowing Water ◽

Transmission Electron ◽

Deposit Layer

A problem was presented to observe the packing densities of deposits of sub-micron corrosion product particles. The deposits were 5-100 mils thick and had formed on the inside surfaces of 3/8 inch diameter Zircaloy-2 heat exchanger tubes. The particles were iron oxides deposited from flowing water and consequently were only weakly bonded. Particular care was required during handling to preserve the original formations of the deposits. The specimen preparation method described below allowed direct observation of cross sections of the deposit layers by transmission electron microscopy.The specimens were short sections of the tubes (about 3 inches long) that were carefully cut from the systems. The insides of the tube sections were first coated with a thin layer of a fluid epoxy resin by dipping. This coating served to impregnate the deposit layer as well as to protect the layer if subsequent handling were required.

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Application of a Simple Cold Stub to the Direct Observation of Frozen Hydrated Sand

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100071508 ◽

1973 ◽

Vol 31 ◽

pp. 212-213

Author(s):

John M. Wehrung ◽

Richard J. Harniman

Keyword(s):

United States ◽

Surface Water ◽

Direct Observation ◽

Controlled Study ◽

Clay Particles ◽

Organic Debris ◽

Rock Formations ◽

Water Tables ◽

Permeable Rock ◽

Natural Means

Water tables in aquifer regions of the southwest United States are dropping off at a rate which is greater than can be replaced by natural means. It is estimated that by 1985 wells will run dry in this region unless adequate artificial recharging can be accomplished. Recharging with surface water is limited by the plugging of permeable rock formations underground by clay particles and organic debris.A controlled study was initiated in which sand grains were used as the rock formation and water with known clay concentrations as the recharge media. The plugging mechanism was investigated by direct observation in the SEM of frozen hydrated sand samples from selected depths.

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Direct Observation of the Diffusionless β → β + ω Transformation in Titanium Alloys

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100064669 ◽

1971 ◽

Vol 29 ◽

pp. 122-123

Author(s):

N. E. Paton ◽

D. de Fontaine ◽

J. C. Williams

Keyword(s):

Electron Microscope ◽

Titanium Alloys ◽

Direct Observation ◽

Dark Field ◽

X Ray Diffraction ◽

Resistivity Measurements ◽

Selected Area Electron Diffraction ◽

Ti Alloys ◽

Thin Foils ◽

Field Device

The electron microscope has been used to study the diffusionless β → β + ω transformation occurring in certain titanium alloys at low temperatures. Evidence for such a transformation was obtained by Cometto et al by means of x-ray diffraction and resistivity measurements on a Ti-Nb alloy. The present work shows that this type of transformation can occur in several Ti alloys of suitable composition, and some of the details of the transformation are elucidated by means of direct observation in the electron microscope.Thin foils were examined in a Philips EM-300 electron microscope equipped with a uniaxial tilt, liquid nitrogen cooled, cold stage and a high resolution dark field device. Selected area electron diffraction was used to identify the phases present and the ω-phase was imaged in dark field by using a (101)ω reflection. Alloys were water quenched from 950°C, thinned, and mounted between copper grids to minimize temperature gradients in the foil.

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