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A high-pressure NMR probehead for measurements at 400 MHz (1994)

Zahl, Achim ; Neubrand, Anton ; Aygen, Sitke ; [et al.]

[S.l.] : American Institute of Physics (AIP)

Review of Scientific Instruments 65 (1994), S. 882-886

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ISSN: 1089-7623

Source: AIP Digital Archive

Topics: Physics , Electrical Engineering, Measurement and Control Technology

Notes: A new high-pressure NMR probehead designed for a 400 MHz widebore NMR spectrometer is described. For the first time, the electrical leads of the rf circuit, the tubes for the thermostating liquid and the high-pressure fluid, as well as the wires of the Pt-100 resistor for temperature control, are all fitted at the bottom of the high-pressure vessel. The sample can easily be removed through a top plug, which allows a relatively fast exchange of the sample. A rather simple design leads to a low-cost construction. The high-pressure vessel and the rf circuit are placed inside a standard probehead jacket, such that the high-pressure probehead can be fitted into the superconducting magnet in the same way as a commercial probehead.

Type of Medium: Electronic Resource

URL: http://dx.doi.org/10.1063/1.1144916

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A Spectroscopic and Mechanistic Study of the Enolization and Diol Formation of Hexafluoroacetylacetone in the Presence of Water and Alcohol (1989)

Aygen, Sitke ; van Eldik, Rudi

Weinheim : Wiley-Blackwell

Berichte der deutschen chemischen Gesellschaft 122 (1989), S. 315-320

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ISSN: 0009-2940

Keywords: Acetylacetone, hexafluoro- ; Diol formation / Enolization ; Chemistry ; Inorganic Chemistry

Source: Wiley InterScience Backfile Collection 1832-2000

Topics: Chemistry and Pharmacology

Description / Table of Contents: Eine spektroskopische und mechanistische Untersuchung der Enolisierung und Diol-Bildung von Hexafluoracetylaceton in Gegenwart von Wasser und AlkoholDie Reaktionen von Hexafluoracetylaceton (Hfac) (6) mit Wasser, Methanol, Ethanol und Isopropylalkohol wurde im einzelnen anhand von 1H-, 13C-, 17O-, 19F-NMR- und UV-VIS-Spektroskopie untersucht. Dabei konnten die Zwischen- und Reaktionsprodukte bei der Enolisierung und Diol-Bildung spektroskopisch identifiziert werden. Die vorgeschlagenen Reaktionswege werden unter Bezug auf früher in der Literatur berichtete Daten diskutiert. Ein wichtiges Ergebnis dieser Untersuchung ist der direkte Nachweis für die Bildung der Addukt-Spezies Hfac(OH)4 (10), Hfac(OMe)2 (13a) und Hfac(OEt)2 (13b).

Notes: The reactions of hexafluoroacetylacetone (hfac) (6) with water, methanol, ethanol, and isopropyl alcohol were studied in detail using 1H-, 13C-, 17O-, 19F-NMR, und UV-VIS spectroscopy. The reported spectra enable the identification of intermediate and product species, and allow a mechanistic analysis of the enolization and diol formation. The suggested mechanisms are discussed with reference to earlier data reported in the literature. An important feature of this study is the direct evidence presented for the formation of the adduct species hfac(OH)4 (10), hfac(OMe)2 (13a), and hfac(OEt)2 (13b).

Additional Material: 6 Ill.