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Cement paste microporosity analysis: a comparison of different experimental techniques

Bednarska Dalia, Koniorczyk Marcin

Technical Transactions

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2019

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Vol. 116, iss. 9

71--80

EN

Microstructure defines almost all material physical properties of a substance. Thus, its proper identification is essential for the assessment of material durability. Porous materials constitute the vast majority of those applied in civil engineering. The most important parameters describing a porous structure are the specific surface area, the shape and volume of pores and the pore size distribution. There are several methods which provide such results; however, each of them has some drawbacks. The main purpose of this paper is to compare results obtained by means of various methods commonly applied to the investigation of microstructure. These methods are mercury intrusion porosimetry (MIP), low temperature sorption of nitrogen and thermoporometry (TPM). The experimental research is conducted on aluminium oxide, which is characterised by unimodal pore size distribution and hardened cement paste prepared using portland cement (CEM I 42.5R with water-cement ratio equal to 0.5. The results obtained by the above-mentioned methods are thoroughly described and compared in this paper. Each of the presented approaches has some limitations; therefore, in order to receive a reliable description of porous microstructure, one has to apply at least two different experimental methods.

PL

Wśród materiałów budowlanych przeważającą większość stanowią materiały porowate. Dokładna znajomość mikrostruktury jest kluczowa w ocenie ich wytrzymałości i trwałości. Istnieje wiele metod eksperymentalnych służących do analizy struktur porowatych. W niniejszym opracowaniu porównane zostały następujące techniki: porozymetria rtęciowa (MIP), niskotemperaturowa adsorpcja azotu oraz termoporometria (TPM). Badaniom eksperymentalnym poddano dwa materiały. Pierwszy z nich, tlenek glinu, jest materiałem referencyjnym o unimodalnym rozkładzie porów. Zgodnie z deklaracją producenta dominująca średnica porów wynosi 7.3 nm. Drugim zastosowanym materiałem jest zaczyn cementowy przygotowany na bazie cementu portlandzkiego CEM I 42,5R. Stwardniały zaczyn charakteryzuje się skomplikowanym rozkładem porów. Opisane techniki analizy mikrostruktury są komplementarne. Aby uzyskać wiarygodny opis struktury wewnętrznej materiałów o skomplikowanym rozkładzie porów należy zastosować co najmniej dwie metody badawcze.

2

Application of Thermoporometry Based on Convolutive DSC to Investigation of Mesoporosity in Cohesive Soils

Kozłowski T., Babiarz I., Grobelska E.

Archives of Hydro-Engineering and Environmental Mechanics

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2010

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Vol. 57, nr 3-4

199-218

EN

In the method of thermoporometry, the characterization of pore space is done by analysis of thermal effects associated with freezing and melting of a liquid in the pores of the material under investigation. Thermoporometry seems particularly well suited to studies of wet porous samples in cases where the process of drying itself is able to destroy the original microstructure, as is the cohesive soils containing montmorillonite. In the paper, a variant of thermoporometry is given in which the blurred calorimetric peak is processed by use of a stochastic-convolutive analysis. As a result, a "sharp" thermogram of real thermal effects is obtained which can be easily transformed into a pore distribution curve. The preliminary results, obtained for samples of three monoionic montmorillonites at different water contents, indicate a greater resolution, sensitivity and precision than the classical thermoporometry using an unprocessed DSC signal. Phenomena corresponding to swelling have been detected in two individual regions on the differential pore distribution curves. The first is a dense spectrum for pores less than 15 nm. The second is a single peak for pores greater than 15 nm. Between the two regions the distribution decays to zero. Apparently, the point of the single peak maximum depends on the total water content, shifting rightward with increasing w. For the region below 20 nm, a strong effect of the kind of exchangeable cation can be observed. The results suggest swelling in the form with bivalent cations (Ca-montmorillonite) and contraction in the form with monovalent cations (Na- and K-montmorillonite).

3

Termoporymetria makroporowatych kationitów sulfonowych

Balcerowiak W., Kulesza K.

Przemysł Chemiczny

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2007

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T. 86, nr 5

382-385