A direct method of quantification of maximal chemisorption of 3-aminopropylsilyl groups on silica gel using DRIFT spectroscopy

Bukleski, Miha; Ivanovski, Vladimir; Hey‐Hawkins, Evamarie

doi:10.1016/j.saa.2015.04.026

Cited by 12 publications

(10 citation statements)

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“…The obtained results are in agreement with our previous results, employing a direct DRIFT method and carbon elemental analysis [27]. The indirect method for determination of the maximal amount of the chemisorbed APS fragments on the silica gel surface employs easier experimental methodology than the direct DRIFT technique in the sense that it does not require inert conditions during the sample preparation for the IR recording and for the recording itself.…”

Section: Introductionsupporting

confidence: 91%

“…Using two samples with higher starting w/w APTMS of 25.16 % and 29.80 %, the average w/w APTMS value at maximum APS chemisorptions was found to be 19.04 %. According to the BET surface value of 589 m 2 /g for the silica gel [27,29], the calculated adsorption for APS was found to be 2.23 μmol m -2 . This value is the same as the one obtained by the direct DRIFT method 2.23 μmol m -2 and very close to the one obtained from elemental analysis 2.22 μmol m -2 [27].…”

Section: Discussionmentioning

confidence: 99%

“…According to the BET surface value of 589 m 2 /g for the silica gel [27,29], the calculated adsorption for APS was found to be 2.23 μmol m -2 . This value is the same as the one obtained by the direct DRIFT method 2.23 μmol m -2 and very close to the one obtained from elemental analysis 2.22 μmol m -2 [27]. These results show that it is possible using an indirect IR transmission method to obtain the chemisorbed amount of adsorbent for the irreversible chemical reaction of APTMS on the silica gel.…”

Section: Discussionmentioning

confidence: 99%

“…unreacted average amount of APTMS per gram silica gel (Table 3) and the starting amount of APTMS for the functionalization of the silica gel (Table 2), the w/w APTMS at which a maximum APS load occurred was calculated (Table 4). It was also possible to calculate the concentration of APS on the silica gel surface (2.23 μmol m -2 ), knowing that the molar ratio of APTMS to APS is 1 and the BET surface of the silica gel (589 m 2 /g, [27,29]) (Table 4). Previous experiments performed on the same samples, but using a direct method of quantification based on DRIFT technique, led to the same value of 2.23 μmol m -2 adsorption, while carbon elemental analyses gave 2.22 μmol m -2 [27].…”

Section: Assessing the Maximum Aps Loadmentioning

confidence: 99%

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Indirect quantitative IR assessment of maximal monomolecular deposition of 3-aminopropyltrimethoxysilane on silica gel surface

Bukleski

Ivanovski

2014

Maced. J. Chem. Chem. Eng.

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Quantification of the amount of maximum loaded 3-aminopropylsilyl (APS) on a thermally pretreated silica gel (600 ºC) was performed using IR spectroscopy. Finding the maximum load through a construction of a Langmuir isotherm was not possible due to the irreversibility of the chemisorption reaction. The method used in this work was based on the analysis of the toluene solution on the quantity of the non-reacted 3-aminopropyltrimethoxysilane (APTMS) after the saturation of the silica gel surface with APS. The process of chemisorption was monitored via the increasing band intensity of (CH 2 ), (NH 2 ), and (NH 2 ) modes of the adsorbent and decreasing (OH) band intensity characteristic for the free isolated OH groups of silica gel using DRIFT spectroscopy. The results on maximum adsorption are in line with those previously obtained, using carbon elemental analysis and a direct DRIFT method.Keywords: 3-aminopropyltrimethoxysilane (APTMS); chemisorption; DRIFT spectra; modified silica gel ИНДИРЕКТНО КВАНТИТАТИВНО ОПРЕДЕЛУВАЊЕ МАКСИМАЛНА МОНОМОЛЕКУЛАРНА ДЕПОЗИЦИЈА НА 3-АМИНОПРОПИЛТРИМЕТОКСИСИЛАН НА ПОВРШИНАТА ОД СИЛИКАГЕЛ СО ИНФРАЦРВЕНА СПЕКТРОСКОПИЈАКвантификацијата на максимално нафатеното количество 3-аминопропилсилил (APS) на температурно активиран силикагел (600 ºC) беше спроведена со помош на инфрацрвена спектроскопија. Определувањето на максимално нафатеното количество преку конструкција на Лангмјурова изотерма не е можно како резултат на иреверзибилноста на хемиската реакција. Користениот метод во оваа работа беше базиран на анализа на растворот од толуен во однос на содржината на неизреагиран 3-аминопропилтриметоксисилан (APTMS) по заситувањето на површината на силикагелот со групи на APS. Процесот на хемисорпција беше следен преку зголемувањето на интензитетот на лентите од модовите на(CH 2 ), (NH 2 ) и (NH 2 ) од атсорби-раните молекули и намалувањето на интензитетот на модот(OH) од слободните, т.е. изолирани OH-групи од силикагелот, со помош на DRIFT спектроскопијата. Добиените резултати за максималната атсорпција се во согласност со претходно добиените од елементарна анализа и со оние добиени со примена на директниот DRIFT-метод.Клучни зборови: 3-аминопропилтриметоксисилан (APTMS); хемисорпција; DRIFT спектри; модифициран силика гел M. Bukleski, V. Ivanovski Maced.

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Section: Introductionsupporting

confidence: 91%

Section: Discussionmentioning

confidence: 99%

Section: Discussionmentioning

confidence: 99%

Section: Assessing the Maximum Aps Loadmentioning

confidence: 99%

See 2 more Smart Citations

Indirect quantitative IR assessment of maximal monomolecular deposition of 3-aminopropyltrimethoxysilane on silica gel surface

Bukleski

Ivanovski

2014

Maced. J. Chem. Chem. Eng.

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“…It is important that the specular reflectance is reduced to a minimum because it distorts the DRIFT spectrum and lowers the band intensities [47]. During the last years, it has become the most effective technique for studying the processes taking place at the gas-solid interface [48].…”

Section: Applications Of Molecular Spectroscopy To Current Research Imentioning

confidence: 99%

Fourier Transform Infrared and Raman Characterization of Silica-Based Materials

Capeletti¹,

Zimnoch²

2016

Applications of Molecular Spectroscopy to Current Research in the Chemical and Biological Sciences

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Fourier Transform Infrared and Raman are powerful techniques to evaluate silica and hybrid silica structure. It is possible to evaluate the silica network formation along the hydrolysis and condensation reactions in terms of siloxane rings formation and Si-O(-Si) angle deformation due to the introduction of organic groups, the employed synthetic route or encapsulated species interaction. The siloxane four-or six-membered rings imply in a more rigid or flexible network, respectively, in order to accommodate the organic groups. A structural analysis of the materials is of high importance, since interactions between the encapsulated molecules and the matrix are critical for the device performance, such as sensors. This type of device needs the permeation of an analyte to activate the encapsulated receptor molecules inside the silica structure. Fourier transform infrared spectrometry can be also used to determine parameters of the silica network as a function of the hydrophilicity/hydrophobicity degree and the siloxane ring structure with respect to thin film porosity. This silica structural analysis is reviewed along the text in a tentative of better exploring the data resulting from these powerful techniques. In addition, the functionalization of silica structures by the use of organoalkoxysilanes, which is important to the creation of high-specific materials, can be well described by these two complementary techniques. The Si-C bonds and the maintenance of the organic substituents such as methyl, octyl, octadecyl, vinyl, phenyl, aminopropyl, mercaptopropyl, isocyanatopropyl, iodopropyl, chloropropyl and glicydoxypropyl could be evaluated after the sol-gel synthesis process. The literature regarding silica vibrational spectroscopy is also explored creating a data bank of wave numbers for the most important bonds for different types of silica and hybrid silica materials obtained by different synthetic routes.

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Elucidating the interaction between polar alkoxysilane-modified silicate glass and ionic surfactant in the obtainment of hydrophobic transparent film

Ivanovski,

Viscusi,

Liparoti

et al. 2024

Colloids and Surfaces A: Physicochemical and Engineering Aspect

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A direct method of quantification of maximal chemisorption of 3-aminopropylsilyl groups on silica gel using DRIFT spectroscopy

Cited by 12 publications

References 33 publications

Indirect quantitative IR assessment of maximal monomolecular deposition of 3-aminopropyltrimethoxysilane on silica gel surface

Indirect quantitative IR assessment of maximal monomolecular deposition of 3-aminopropyltrimethoxysilane on silica gel surface

Fourier Transform Infrared and Raman Characterization of Silica-Based Materials

Elucidating the interaction between polar alkoxysilane-modified silicate glass and ionic surfactant in the obtainment of hydrophobic transparent film

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