Christy Alfred A, Egeberg Per K
Department of Natural Sciences, Faculty of Mathematics and Sciences, Agder University College, Serviceboks 422, N-4604 Kristiansand, Norway.
Analyst. 2005 May;130(5):738-44. doi: 10.1039/b501895c. Epub 2005 Apr 8.
Concentration of silanol groups on silica gel surface has been quantitatively determined using the deuterium exchange method. Simple and effective procedures have been used in pre-sample drying, deuterium exchange and extraction of resulting isotopic mixture from the exchange reaction. Each of four silica gel samples with varying surface area has been subjected to pre-drying to remove adsorbed water and then quantitatively mixed with deuterium oxide in a steel bomb for isotopic exchange. The resulting D(2)O/water mixture was then extracted by applying high pressure using infrared pellet press. The infrared spectrum of the isotopic mixture was measured and the composition was then determined by a multivariate calibration model established between infrared profiles of water in D(2)O standard mixtures and their composition. The results show that the silanol group concentration determined agrees with the values reported in the literature.
采用氘交换法对硅胶表面硅醇基团的浓度进行了定量测定。在样品预干燥、氘交换以及从交换反应中提取所得同位素混合物的过程中，使用了简单有效的程序。对四个具有不同表面积的硅胶样品分别进行预干燥以去除吸附水，然后在钢弹中与重水进行定量混合以进行同位素交换。接着使用红外压片机施加高压来提取所得的D₂O/水混合物。测量了同位素混合物的红外光谱，然后通过在D₂O标准混合物中水的红外谱图与其组成之间建立的多元校准模型来确定其组成。结果表明，所测定的硅醇基团浓度与文献报道的值相符。
