NMR cryoporometry with octamethylcyclotetrasiloxane as a probe liquid. Accessing large pores

Vargas-Florencia, Dulce; Petrov, Oleg V.; Furó, István

doi:10.1016/j.jcis.2006.09.054

Cited by 40 publications

(64 citation statements)

References 48 publications

(70 reference statements)

Supporting

Mentioning

Contrasting

Order By: Relevance

“…Recently, NMR cryoporometry has been applied to the macropore range [42]. By using octamethylcyclotetrasiloxane as a probe liquid, it seems possible to study the pore size range from 10 nm up to 1 μm.…”

Section: Version Based On Nuclear Magnetic Resonance: "Nmr Cryoporomementioning

confidence: 99%

Liquid intrusion and alternative methods for the characterization of macroporous materials (IUPAC Technical Report)

Rouquérol

Baron

Denoyel

et al. 2011

Pure and Applied Chemistry

187

View full text Add to dashboard Cite

This document deals with the characterization of porous materials having pore widths in the macropore range of 50 nm to 500 μm. In recent years, the development of advanced adsorbents and catalysts (e.g., monoliths having hierarchical pore networks) has brought about a renewed interest in macropore structures. Mercury intrusion-extrusion porosimetry is a well-established method, which is at present the most widely used for determining the macropore size distribution. However, because of the reservations raised by the use of mercury, it is now evident that the principles involved in the application of mercury porosimetry require reappraisal and that alternative methods are worth being listed and evaluated. The reliability of mercury porosimetry is discussed in the first part of the report along with the conditions required for its safe use. Other procedures for macropore size analysis, which are critically examined, include the intrusion of other non-wetting liquids and certain wetting liquids, capillary condensation, liquid permeation, imaging, and image analysis. The statistical reconstruction of porous materials and the use of macroporous reference materials (RMs) are also examined. Finally, the future of macropore analysis is discussed.

show abstract

Section: Version Based On Nuclear Magnetic Resonance: "Nmr Cryoporomementioning

confidence: 99%

Liquid intrusion and alternative methods for the characterization of macroporous materials (IUPAC Technical Report)

Rouquérol

Baron

Denoyel

et al. 2011

Pure and Applied Chemistry

187

View full text Add to dashboard Cite

show abstract

“…In proton-exchange membranes, water is a native constituent of the system and is therefore the natural choice as probe liquid. NMR cryoporometry can explore a rather wide range of pore sizes (~nm up to~lm [18]), which makes it a technique complementary to more traditional analytical tools such as (i) SAXS and small angle neutron scattering (SANS), which are in most studies limited to a narrow scattering-vector space, i.e. only small domains are detectable and (ii) surface characterisation methods such as transmission electron microscopy (TEM) and atomic force microscopy (AFM) [9].…”

Section: Introductionmentioning

confidence: 99%

Pore Size Distribution and Water Uptake in Hydrocarbon and Perfluorinated Proton‐Exchange Membranes as Studied by NMR Cryoporometry

et al. 2008

Self Cite

View full text Add to dashboard Cite

Sulfonated polysulfone (sPSU) membranes were analysed by nuclear magnetic resonance (NMR) cryoporometry, conventional gravimetric water uptake measurements as well as by differential scanning calorimetry (DSC). NMR cryoporometry is based on the relation between the pore size and the melting point depression of the pore‐filling liquid, i.e. water in fuel cell membranes; thus providing a relation between the amount of molten water and the temperature shift, i.e. the pore size, in hydrated membranes. An sPSU membrane with high ion‐exchange capacity (IEC 1.45 mequiv. g–1) possessed a significant amount of large pores after hydrothermal pre‐treatment at 80 °C, which was related to its high hydrophilicity and low resistance towards swelling. An sPSU membrane with low IEC (0.95 mequiv. g–1) showed a significant fraction of small pores (r ∼ 1 nm) after hydrothermal pre‐treatment at 80 °C, implying a controlled water uptake of the membrane. NMR cryoporometry was also carried out on Nafion membranes, the results were found to be in agreement with the water uptake measurements and revealed a pore size distribution peak at r ∼ 1 nm. The NMR cryoporometry, gravimetric water uptake and DSC results are also discussed in terms of the state of the water and methodological differences.

show abstract

“…Pore size distribution was measured by three different experimental techniques, i.e., mercury porosimetry, 1 H NMR cryoporometry [19][20][21][22] and nitrogen gas adsorption technique.…”

Section: Pore Size Distribution Porosity and Specific Surface Areamentioning

confidence: 99%

“…The pore size distribution was also measured by the 1 H NMR cryoporometry as follows [19][20][21][22]. The principle is the melting temperature depression in small pores.…”

Section: Pore Size Distribution Porosity and Specific Surface Areamentioning

confidence: 99%

“…Therefore, the pore characterization with the changes of calcination temperature and r c in fractal porous-silica should be systematically investigated. In this article, we report the first experimental results on the pore characterization of the fractal porous-silica samples with the changes of T cal and r c over an extremely wide scale range from 1 nm to 100 m by the set of different techniques of SEM observation, mercury porosimetry, 1 H NMR cryoporometry [19][20][21][22] and nitrogen gas adsorption technique. We will address a correlation between the pore characterization and the fractal geometries.…”

Section: Introductionmentioning

confidence: 99%

See 1 more Smart Citation

Characterization and structural investigation of fractal porous-silica over an extremely wide scale range of pore size

Ono

Mayama

Furó

et al. 2009

Journal of Colloid and Interface Science

View full text Add to dashboard Cite

We have succeeded in creating Menger sponge-like fractal body, i.e., porous-silica samples with Menger sponge-like fractal geometries, by a novel template method utilizing template particles of alkylketene dimer (AKD) and a sol-gel synthesis of tetramethyl orthosilicate (TMOS). We report here the first experimental results on characterization and structural investigations of the fractal porous-silica samples prepared with various conditions such as calcination temperature and packing condition of the template particles. In order to characterize the fractal porous-silica samples, pore volume distribution, porosity and specific surface area were measured over an extremely wide scale from 1 nm to 100 m by means of mercury porosimetry, 1 H NMR cryoporometry, and nitrogen gas adsorption experiments together with direct evaluations of cross-sectional fractal dimension D cs , size limits of D cs . We have found that the pore volume distribution and specific surface area of the fractal porous-silica samples can be discussed in terms of different fractal porous structures at different scale regions.

show abstract

NMR cryoporometry with octamethylcyclotetrasiloxane as a probe liquid. Accessing large pores

Cited by 40 publications

References 48 publications

Liquid intrusion and alternative methods for the characterization of macroporous materials (IUPAC Technical Report)

Liquid intrusion and alternative methods for the characterization of macroporous materials (IUPAC Technical Report)

Pore Size Distribution and Water Uptake in Hydrocarbon and Perfluorinated Proton‐Exchange Membranes as Studied by NMR Cryoporometry

Characterization and structural investigation of fractal porous-silica over an extremely wide scale range of pore size

Contact Info

Product

Resources

About