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Examples of Hydrothermal Titration and Real Time X-Ray Diffraction in the Synthesis of Open Frameworks

1996/01/01 by John B. Parise, J. B. Parise, K. Tan +6 · 1 citation
Chemistry · Environmental Science · #Chemical Synthesis and Characterization #Metal-Organic Frameworks: Synthesis and Applications #Zeolite Catalysis and Synthesis

paper · doi:10.1557/proc-453-103

crossref issued 1996/01/01 · crossref published 1996/01/01 · crossref published-print 1996/01/01 · openalex publication_date 1996/01/01 · crossref published-online 2011/02/15 · crossref created 2011/04/05 · crossref deposited 2021/02/24 · crossref indexed 2022/04/05 · openalex created_date 2025/10/10 · openalex updated_date 2026/07/28

Abstract

Abstract Hydrothermal titration (HTT) techniques represent a new synthetic strategy for the production of open frameworks. As an example, initial digestion of amorphous GeS 2 in the presence of tetraethyl ammonium hydroxide (TEAOH) at 100°C is followed by injection of Ag + into this mixture to condense the [Ge 4 S 10 ] 4− clusters and form a framework consisting of 8-ring channels bounded by alternating GeS-clusters and Ag + . The rational use of this apparatus depends upon determining the timing of injection. Insight into the changes occurring during reactant digestion is provided by real time synchrotron X-ray powder diffraction. Changes in the the system dimethylamine-Sb-S have been followed in real time at different temperatures. The transformation from mixtures of DMA, Sb and S to the known open phase DMA-SbS-SB8 was followed by observing monochromatic X-ray scattering detected on an imaging plates over a 8 hr period with one continuous exposure.

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