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Facile determination of the degree of modification of ordered mesoporous silica by liquid phase NMR
Microporous and Mesoporous Materials ( IF 5.2 ) Pub Date : 2018-09-04 , DOI: 10.1016/j.micromeso.2018.08.034
Andreas G. Thomé , Frank Schroeter , Patrick Bottke , Jatuporn Wittayakun , Frank Roessner

A new and facile analytical method to assess the amount of organic groups that are linked to the surface of ordered mesoporous silica (OMS) is proposed. The quantity of adsorbed compounds on OMS could also be studied as well as the amount of silanol groups within certain limits. A small amount of the OMS of interest is dissolved in a small volume of NaOD in D2O and a defined amount of a reference compound is added. Subsequently, the solution is analyzed by liquid phase NMR. The degree of modification can be inferred quantitatively from the 1H-spectrum. The high accuracy and the analysis time compared to solid-state 1H and 13C MAS NMR are the main benefits of this method. The findings are correlated with XRD, N2-sorption, DRIFTS, TGA and MAS NMR data.



中文翻译:

液相NMR轻松测定有序中孔二氧化硅的改性度。

提出了一种新的简便的分析方法,用于评估与有序介孔二氧化硅(OMS)表面相连的有机基团的数量。还可以研究在OMS上吸附的化合物的量以及在一定范围内的硅烷醇基团的量。将少量感兴趣的OMS溶解在D 2 O中的少量NaOD中,并添加确定量的参比化合物。随后,通过液相NMR分析溶液。可以从1 H光谱定量推断出修饰的程度。与固态1 H和13 C MAS NMR相比,高精度和分析时间是该方法的主要优点。研究结果与XRD,N 2相关吸附,DRIFTS,TGA和MAS NMR数据。

更新日期:2018-09-04
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