Adsorptionseigenschaften und Oberflächenstruktur von Quarzpulvern

This review is intended to summarize current knowledge on chemically bonded stationary phases. Their preparation and effect on chromatographic processes in GC and HPLC are described and the complex separation mechanism on these phases is discussed.

Chemically bonded stationary phases for gas and high performance liquid chromatography

Die Bindung des Wassers in verschiedenen Verbindungen der Systeme Al2O3/H2O, SiO2/H2O und Fe2O3/H2O wird mit Hilfe von Ultrarotabsorptionsmessungen studiert.



Durch Dehydration aus Aluminiumhydroxyden entstandene Aluminiumoxyde enthalten noch Wasser, das in Form von OH-Gruppen im Gitter vorliegt.



Bei der Hydrolyse von Kieselsauretetraathylester gewinnt man Praparate, die je nach Vorbehandlung einen wesentlichen Teil oder fast alles Wasser als OH-Gruppen gebunden enthalten.



Die aus Eisen(III)-salzlosungen mit OH-Ionen gefallten braunen, amorphen Produkte haben in ihrem Gerust das Wasser als OH-Gruppe eingebaut. Mit zunehmender Alterung oder durch Erhitzen tritt Wasserabgabe zu hoher kondensierten Hydroxyden ein.



Es werden zwei neue Gruppen von Hydroxyden unterschieden: 1. Kondensierte Hydroxyde, 2. Nichtstochiometrische Hydroxyde.



The nature of water in several compounds of the systems Al2O3H2O, SiO2H2O and Fe2O3H2O has been studied by investigation of the infra-red absorption.



Aluminium oxides prepared by dehydration of aluminium hydroxides still contain OH-groups. Hydrolysis of silicic acid tetraethyl ester yields products in which most or all of the bound water is water of constitution, too. Iron(III) oxide-hydrates precipitated in the usual manner also contains water in form of OH-groups; on crystallization or by heating the precipitates, loss of water occurs with formation of higher condensed hydroxides.



Two new types of hydroxides are distinguished: condensed and nonstoichiometric hydroxides.

Zur Bindung des Wassers in den Systemen Al2O3/H2O, SiO2/H2O und Fe2O3/H2O

The silanol groups of a silica preparation were determined by ignition and by reaction with LiAlH, (244meq. SiOH per 100g silica). Part of these groups reacted with organic reagents forming organic derivatives of silica with SiOC bonds.

Organische Derivate des Silikagels mit SiOC-Bindung I†

Die Reaktion von flussigem (CH3)3SiCl mit feinkornigem porosem Silicagel wurde bei 20°C experimentell untersucht. Das Kapillarwasser des Silicagels wird unter Bildung fluchtiger Hydrolyseprodukte verbraucht. Chemisch gebundenes Wasser fuhrt zu einer Gewichtsvermehrung des Bodenkorpers und zur Erhohung seines Gluhruckstandes (SiO2). Daraus ergibt sich die Moglichkeit, strukturelle Veranderungen des Silicagels beim Erhitzen und damit verbundene Anderungen seines Reaktionsvermogens mit Wasser durch gravimetrische Analyse zu verfolgen. Es wird diskutiert, wie weit die Analysenergebnisse mit Hilfe der Gleichung (CH3)3SiCl + HOSi(O/2)3 (CH3)3SiOSi(O/2)3 + HCl beschrieben werden durfen.

Umsetzung von Trimethylsiliciummonochlorid mit Silicagel

Notizen: Oxydationsprodukte des Siloxens und ihre Charakterisierung durch Fluoreszenzindikatoren

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Notizen: Oxydationsprodukte des Siloxens und ihre Charakterisierung durch Fluoreszenzindikatoren