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For many microstructural studies it is necessary to “stop” cement hydration—to remove free water. This paper describes the results of a round robin test on the impact of hydration stoppage methods on the composition of hydrated cements. A regular and a fly ash blended Portland cement hydrated for 90 days were selected. Ten laboratories participated in the round robin test. Four common hydration stoppage methods were studied: (1) oven drying at 105 °C, (2) solvent exchange by isopropanol, (3) vacuum drying and (4) freeze drying. After the stoppage of hydration powder samples were studied by thermogravimetry (TG) and X-ray diffraction (XRD). Bound water and Ca(OH)2 content were determined based on the TG data. Portlandite and ettringite content were quantified by Rietveld analysis of the XRD data. The goal was to establish interlaboratory reproducibility and to identify the best available protocols for research and standardization purposes. Based on the results of the round robin test three recommendations are made. (1) Oven drying at 105 °C is not recommended. This dehydrates, alters and decomposes calcium aluminate hydrates significantly more than other methods and often produced carbonation artefacts. (2) Isopropanol exchange is the most appropriate hydration stoppage method for the study of the complete hydrate assemblage of cements, including calcium aluminate hydrates such as ettringite and AFm phases. (3) For quantification of portlandite (Ca(OH)2) all tested hydration stoppage protocols are satisfactory, with the exception of oven drying.

This recommendation is an outcome of the work carried out by a working group within the RILEM Technical Committee 238-SCM “Supplementary Cementitious Materials”. The working group studied the effect of supplementary cementitious materials on the pore solution, the microstructure and the hydration product assemblage of hardened Portland cements blended with common supplementary cementitious materials. The recommendation reflects the results of a round robin test programme on common hydration stoppage methods in 10 participating laboratories. Among four different methods tested, solvent exchange by isopropyl alcohol (isopropanol) gave the best results in terms of preservation of the cement hydrate assemblage and overall reproducibility of the results [1]. The current protocol is developed based on best laboratory practices of the participating laboratories and literature reports [2–4]. The presented hydration stoppage protocol is recommended for the study of Portland cement-based hydrate assemblages by common material characterization techniques such as thermogravimetry and X-ray powder diffraction.

A primary aim of RILEM TC 267-TRM: “Tests for Reactivity of Supplementary Cementitious Materials (SCMs)” is to compare and evaluate the performance of conventional and novel SCM reactivity test methods across a wide range of SCMs. To this purpose, a round robin campaign was organized to investigate 10 different tests for reactivity and 11 SCMs covering the main classes of materials in use, such as granulated blast furnace slag, fly ash, natural pozzolan and calcined clays. The methods were evaluated based on the correlation to the 28 days relative compressive strength of standard mortar bars containing 30% of SCM as cement replacement and the interlaboratory reproducibility of the test results. It was found that only a few test methods showed acceptable correlation to the 28 days relative strength over the whole range of SCMs. The methods that showed the best reproducibility and gave good correlations used the R3 model system of the SCM and Ca(OH)2, supplemented with alkali sulfate/carbonate. The use of this simplified model system isolates the reaction of the SCM and the reactivity can be easily quantified from the heat release or bound water content. Later age (90 days) strength results also correlated well with the results of the IS 1727 (Indian standard) reactivity test, an accelerated strength test using an SCM/Ca(OH)2-based model system. The current standardized tests did not show acceptable correlations across all SCMs, although they performed better when latently hydraulic materials (blast furnace slag) were excluded. However, the Frattini test, Chapelle and modified Chapelle test showed poor interlaboratory reproducibility, demonstrating experimental difficulties. The TC 267-TRM will pursue the development of test protocols based on the R3 model systems. Acceleration and improvement of the reproducibility of the IS 1727 test will be attempted as well.

Advanced modeling of unsaturated water and contaminant transport in concrete requires knowledge of the unsaturated conductivity (permeability) function and the water retention curve. An assumption of simple Fickian diffusion is not sufficient due to the nonlinear water and contaminant fluxes. The Van Genuchten-Mualem conductivity model, widely used in describing hydraulic properties of soils, is validated by predicting experimental moisture content profiles obtained by nuclear magnetic resonance during simple absorption experiments with concrete cylinders. A new tortuosity parameter is suggested. Analytical methods are extended based on the Van Genuchten-Mualem model, to provide a means of estimating the saturated permeability from the much simpler sorptivity experiment. The predicted permeability is similar to the long-term experimental permeability. This suggests that only the very long-term saturated permeability is suitable for describing unsaturated moisture flux. [PUBLICATION ABSTRACT]

The performance of concrete, in terms of its placeability, physical properties, and its durability, can be enhanced by the use of slag-blended cements or separately added ground granulated blast-furnace slag. It also has advantages for architectural purposes due to the whiteness it imparts to concrete. Properly proportioned and cured slag concretes will control deleterious alkali-silica reactions, impart sulphate resistance, greatly reduce chloride ingress, and reduce heat of hydration. Setting times and early age strengths can be controlled through appropriate proportioning, while later age properties are typically enhanced. CSA and ASTM standards cover both slag-blended cements (CSA A362; ASTM C595; ASTM C1157) and slag as a supplementary cementing material (CSA A23.5; ASTM C989). Since Lafarge introduced the first large-scale slag grinding plant near Hamilton in 1976, slag has become the predominant supplementary cementing material in Ontario. Recently, its availability in the U.S. has expanded dramatically.Key words: blast-furnace slag, concrete performance, supplementary cementing material.

To evaluate measures to prevent alkali-silica reaction (ASR) in concrete and to correlate short-term laboratory tests to longterm performance, an outdoor exposure site was established in Kingston, ON, Canada, in 1991. Alkali-silica reactive aggregate was combined into six concrete mixtures using various cements and supplementary cementitious materials (SCMs). Both unreinforced and reinforced 0.6 x 0.6 x 2 m (24 x 24 x 79 in.) beams, and 0.2 x 1.2 x 4 m (8 x 48 x 158 in.) pavement slabs were instrumented and have been monitored for 20 years. The high-alkali cement concrete cracked at 5 years and low-alkali cement cracked after 12 years. The high-alkali cement was replaced with various amounts of SCMs. Two concretes, containing 50% ground-granulated blastfurnace slag (GGBFS) and a ternary blend of 25% slag plus 3.8% silica fume interground with a high-alkali portland cement, have neither expanded nor cracked. After 14 years, cores were examined petrographically, chloride penetration profiles were made, and chloride diffusion as well as rapid chloride permeability tests, were performed.

This design specification provides minimum requirements for performing a service life evaluation as part of the design process for new structures and implementing the results of the evaluation into the construction phase. This design specification can be used as part of a design-bid-build project, a design-build project, or other project delivery options. The design specification is independent of the specific model or technique used to perform the service life evaluation. Although service life modeling is commonly used to evaluate chloride transport causing corrosion deterioration, the approach outlined in this design specification can be used for any deterioration mechanism that is capable of being modeled. The service life engineer performing the evaluation can either be the prime consultant or a subconsultant. A service life report is produced as part of this specification, documenting the service life evaluation, followed by a service life record report documenting the implementation into the new construction.

In Ontario, two types of alkali-aggregate reaction exist. Each type is evaluated using different tests. Over the past few years, new tests have been introduced to replace some existing test methods. The new tests are faster and more reliable. Preventive measures such as the use of low-alkali cement and supplementary cementing materials, while they are effective, have not been extensively used with reactive aggregate in Ontario. Beneficiation or selective extraction is used with some potentially reactive aggregates.Key words: alkali-aggregate reaction, concrete, cracking, Ontario, structures.

The water retention curve (WRC) is a hydraulic characteristic of concrete required for advanced modeling of water (and thus solute) transport in variably saturated, heterogeneous concrete. Unfortunately, determination by a direct experimental method (for example, measuring equilibrium moisture levels of large samples stored in constant humidity cells) is a lengthy process, taking over 2 years for large samples. A surrogate approach is presented in which the WRC is conveniently estimated from mercury intrusion porosimetry (MIP) and validated by water sorption isotherms. The well-known Barrett, Joyner, and Halenda (BJH) method of estimating the pore size distribution (PSD) from the water sorption isotherm is shown to complement the PSD derived from conventional MIP. This provides a basis for predicting the complete WRC from MIP data alone. The van Genuchten equation is used to model the combined water sorption and MIP results. It is a convenient tool for describing water retention characteristics over the full moisture content range. The van Genuchten parameter estimation based solely on MIP is shown to give a satisfactory approximation to the WRC, with a simple restriction on one of the parameters. [PUBLICATION ABSTRACT]