Infrared Study of the Nature of the Hydroxyl Groups on the Surface of Porous Glass

Low, M. J. D.; Ramasubramanian, N.

doi:10.1021/j100881a006

Cited by 68 publications

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“…In a number of cases it was found that the intensity of the band due to the free silanol groups was essentially unaffected on adsorption of water [29,[36][37][38][39][40][41][42], while in others it definitely decreased [6,[43][44][45][46][47]. In their extensive studies on porous silica glass, Low and Ramasubramanian [17,48,491 show that B-OH groups not only exist on the well-dehydroxylated glass surface but are the main centres of water adsorpttion. A band in the fundamental region at 3,600 cm-1 has been ascribed to molecular water adsorbed on boron.…”

Section: Site Of Adsorptionmentioning

confidence: 99%

Simultaneous determination of the spectroscopic and adsorption isotherms of water on silica

Litvan

Yamasaki

1972

Mat. Constr.

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Section: Site Of Adsorptionmentioning

confidence: 99%

Simultaneous determination of the spectroscopic and adsorption isotherms of water on silica

Litvan

Yamasaki

1972

Mat. Constr.

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“…The adsorbents used were Cab-0-Sil silica1, porous glass2, and fully fluoridated porous glass (2). The porous glass was used for most of the work because of the ease of preparing and handling of the samples.…”

Section: Methodsmentioning

confidence: 99%

“…anisole was subjected to freeze-thaw cycles and was distilled in vacuo. Some minor experimental details are given elsewhere (2). Spectra were recorded with a Perkin-Elmer model 621 spectrometer.…”

Section: Methodsmentioning

confidence: 99%

“…Canadian Journal of Chemistry, 47, 3909 (1969) Bis-2-pyridylglycol(1) (BPG) has already been used as a gravimetric reagent (1) for aluminum(III), beryllium(II), and uranium(V1) and as a spectrophotometric reagent for iron(II1) (2) and cobalt(I1) (3). The present note deals with the studies of copper(I1) complexes of BPG and its 6,6'-dimethyl derivative (2) (DMBPG) using spectrophotometric, conductometric, and pHmetric methods.…”

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Dual interaction of anisole with surface hydroxyls

Low¹,

Cusumano²

1969

Can. J. Chem.

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Infrared spectra were recorded of anisole adsorbed on porous glass which had been dehydroxylated to various extents, on highly dehydroxylated silica, and on fully fluoridated porous glass. Spectra recorded at various surface coverages showed 2 broad bands near 3600 and 3400 cm−1 due to perturbed surface hydroxyls, indicating that the adsorbed anisole was weakly held to the surface in 2 ways. The surface structures and mechanism are discussed.

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“…Recent work has shown that many of the differences in the surface properties of porous glass and pure silica can be attributed to the minority constituents on the glass (1,2). Pure silica is relatively inert, but can be made "active," so that it resembles porous glass in behavior, by impregnating the silica with oxides such as alumina or boria.…”

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Infrared study of the interactions of acetone and siliceous surfaces

McManus¹,

Harano²,

Low³

1969

Can. J. Chem.

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Adsorbed acetone is held to silica surfaces by hydrogen bonds between surface silanols and the acetone carbonyl groups. Acetone is adsorbed by this mechanism on porous glass surfaces but there is also some decomposition, as shown by the increase in surface B-OH groups and by formation of new C-H absorptions at 2984 and 2940 cm-I. Experiments with boron-impregnated silica indicated that the presence of boron in the porous glass can account for this decomposition process. Bands at 1660-1670 and 1650 cm-', observed when acetone and acet0ne-d6, respectively, were adsorbed on either porous glass or boron-impregnated silica, are attributed to v((7=0) of the carbonyl group coordinated with a surface boron atom. The surface hydroxyls of both silica and porous glass could exchange with the deuterium of acetone-d6 via a mechanism involving an en01 intermediate. 47,2545 (1969) Recent work has shown that many of the differences in the surface properties of porous glass and pure silica can be attributed to the minority constituents on the glass (1, 2). Pure silica is relatively inert, but can be made "active," so that it resembles porous glass in behavior, by impregnating the silica with oxides such as alumina or boria. As much of the recent infrared (i.r.) work had been carried out with water (3) and nitrogenous compounds (4-6), it was thought desirable to extend the studies to oxygen-containing adsorbates such as methanol (7) and acetone, so that information would be available on the reactions of adsorbates having different "functional groups". Canadian Journal of Chemistry,The present paper describes our attempts to characterize the interactions of acetone with porous glass and some silicas by i.r. techniques.The acetone -porous glass system has been examined previously (8,9), but the studies were brief. Also, i.r. studies involving adsorbates such as acetone are fraught with difficulty because there is always the possibility that grease may be transported from joints onto the adsorbent surface. In the present experiments we approached this problem by using acetone and acetone-d6 which were purified and stored in a grease-free acetone (Aldrich Chemical Co.) were stored and purified in a section of the apparatus made entirely from glass and Teflon stopcocks. These adsorbates were dried in vacuo over either anhydrous copper or calcium sulfates and degassed by freeze-pumpthaw cycles until no pressure burst was evident on the Pirani gauge. Infrared spectra of acetone and acetone-d6 in both the gas and liquid phase showed excellent agreement with the data of Dellepiane and Overend (10). Corning Grade 7930 porous glass was used in the form of 1 mm-thick plates. Thinner, ground samples (approx. 0.2 mm) were used in some experiments. Other samples were self-supporting discs of Cab-0-Sil (Cab-0-Sil M5 Silica, supplied by G . Cabot, Boston, Mass.), and of Cab-0-Sil impregnated with either 1 % of boron or 1 % of aluminium by the incipient-wetness method. All samples were outgassed in vacuo at 600' for 3 h, heated in 50 Torr oxyge...

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Infrared Study of the Nature of the Hydroxyl Groups on the Surface of Porous Glass

Cited by 68 publications

References 0 publications

Simultaneous determination of the spectroscopic and adsorption isotherms of water on silica

Simultaneous determination of the spectroscopic and adsorption isotherms of water on silica

Dual interaction of anisole with surface hydroxyls

Infrared study of the interactions of acetone and siliceous surfaces

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