scholarly journals Nuclear Magnetic Resonance Spectroscopy for In Situ Monitoring of Porous Materials Formation under Hydrothermal Conditions

Materials ◽  
2018 ◽  
Vol 11 (8) ◽  
pp. 1416 ◽  
Author(s):  
Mohamed Haouas

The employment of nuclear magnetic resonance (NMR) spectroscopy for studying crystalline porous materials formation is reviewed in the context of the development of in situ methodologies for the observation of the real synthesis medium, with the aim of unraveling the nucleation and growth processes mechanism. Both liquid and solid state NMR techniques are considered to probe the local environment at molecular level of the precursor species either soluble in the liquid phase or present in the reactive gel. Because the mass transport between the liquid and solid components of the heterogeneous system plays a key role in the synthesis course, the two methods provide unique insights and are complementary. Recent technological advances for hydrothermal conditions NMR are detailed and their applications to zeolite and related materials crystallization are illustrated. Achievements in the field are exemplified with some representative studies of relevance to zeolites, aluminophosphate zeotypes, and metal-organic frameworks.

Lab on a Chip ◽  
2019 ◽  
Vol 19 (4) ◽  
pp. 641-653 ◽  
Author(s):  
Ian Swyer ◽  
Sebastian von der Ecken ◽  
Bing Wu ◽  
Amy Jenne ◽  
Ronald Soong ◽  
...  

We describe a two-plate digital microfluidic method for interfacing with nuclear magnetic resonance spectroscopy (DMF-NMR) for microscale chemical analysis.


1995 ◽  
Vol 269 (2) ◽  
pp. C318-C322 ◽  
Author(s):  
S. K. Song ◽  
R. S. Hotchkiss ◽  
J. Neil ◽  
P. E. Morris ◽  
C. Y. Hsu ◽  
...  

Fluorine-19-nuclear magnetic resonance (19F-NMR) spectroscopic detection of the NMR-active Ca2+ indicator 5-fluoro-1,2-bis(2-aminophenoxy)ethane-N,N,N',N'-tetraacetic acid (5F-BAPTA) is one method for measuring cytosolic free Ca2+ concentration ([Ca2+]i) and has been used previously to measure [Ca2+]i in isolated cells and perfused organs. The aim of the present investigation was to demonstrate the feasibility of determining [Ca2+]i in vivo and in situ using 19F-NMR and 5F-BAPTA. Experiments were performed on male Sprague-Dawley rats with a surface-coil antenna employed for NMR interrogation. The Ca2+ indicator, 5F-BAPTA, was infused either intravenously (kidney, spleen) or intraventricularly (brain) as a 100 mg/ml solution of the cell-permeant acetoxymethyl ester (5F-BAPTA-AM) in dimethyl sulfoxide. Rats tolerated intravenous infusion without evident change in mean arterial blood pressure. In all tissues examined, kidney, spleen, and brain, [Ca2+]i was approximately 200 nM. To our knowledge, these results represent the first in vivo and in situ determinations of [Ca2+]i employing 19F-NMR.


2018 ◽  
Vol 72 (9) ◽  
pp. 1404-1415
Author(s):  
Xiaoyun Chen ◽  
Donald Eldred ◽  
Jing Liu ◽  
Hsu Chiang ◽  
Xianghuai Wang ◽  
...  

Sol-gels are found in many different scientific fields and have very broad applications. They are often prepared by the hydrolysis and condensation of alkoxysilanes such as trimethoxysilanes, which are commonly used as precursors in the preparation of silsequioxanes via the sol-gel process. The reaction rates of such reactions are influenced by a wide range of experimental factors such as temperature, pH, catalyst, etc. In this study, we combined multiple in situ spectroscopic techniques to monitor the hydrolysis and partial condensation reactions of methyltrimethoxysilane and phenyltrimethoxysilane. A rich set of kinetics information on intermediate species of the hydrolysis reactions were obtained and used for kinetics modeling. Raman and nuclear magnetic resonance (NMR) spectroscopy provided the most information about hydrolysis and NMR provided the most information about condensation. A quantitative method based on Raman spectra to quantify the various transient intermediate hydrolysis products was developed using NMR as the primary method, which can be deployed in the field where it is impractical to carry out NMR measurements.


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