Use of the Falling-Head Method to Assess Permeability of Freshly Mixed Cementitious-Based Materials Downloaded from ascelibrary.org by UNIVERSITY OF PITTSBURGH on 08/01/13. Copyright ASCE. For personal use only; all rights reserved. Joseph J. Assaad 1 and Jacques Harb 2 Abstract: The falling-head method determined using a permeameter cell is commonly used to study permeability (k) of soils and facility of fluids to travel through a solid skeleton. A research program was undertaken to evaluate the suitability of such test for assessing permeability of freshly mixed mortars and concrete. Validation of k values with respect to bleeding and surface settlement responses and correlations with permeability calculated using empirical soil models are established. The falling-head method was found appropriate to assess the effect of mixture composition (i.e., binder content, water-to-cement ratio, and chemical/mineral admixtures) on permeability variations. Concrete incorporating coarse aggregates exhibited greater permeability levels than those determined on mortars. Despite the differences in chemical nature between soil and mortar, the actual k values determined by testing were found to be well correlated to those calculated by using several previously reported empirical soil models. DOI: 10.1061/(ASCE)MT.1943-5533.0000630. © 2013 American Society of Civil Engineers. CE Database subject headings: Mortars; Concrete; Permeability; Settlement; Soils; Cement. Author keywords: Mortar; Concrete; Bleeding; Permeability; Settlement; Soil. Introduction Hydraulic conductivity or simply permeability (k) of freshly mixed cementitious-based materials is a key indicator of hydromechanical properties (i.e., static stability, pumping, formwork pressure, plastic shrinkage) and their evolution with time. Several researchers reported that permeability of fresh concrete can be used to reflect its ability to remain homogeneous during the pumping and forming processes (Browne and Bamforth 1977; Perrot et al. 2009). Mixtures exhibiting lower levels of permeability were found to develop better static stability including lower aggregate segregation and bleeding, together with improved hardened properties such as bonding to embedded reinforcement (Appleby and Wilson 1996; Josserand et al. 2006). Moreover, permeability was reported to largely influence lateral pressure developed by plastic concrete on vertical formworks. Assaad et al. (2009b) found that concrete proportioned with higher cement content and lower water-tocement ratio (w=c) reduced tendency of water to drain out of the material, thus resulting in lower formwork pressure. In addition, concrete permeability affects the rate of capillary pressure buildup during setting, and consequently the susceptibility against plastic shrinkage (Slowik et al. 2008). The approach traditionally used to assess hydraulic conductivity of fresh cementitious-based materials involves applying a given pressure on top of the specimen and measuring the amount of free mixing water that is squeezed out from the bottom surface. 1 Professor of Civil Engineering; R&D Manager, Holderchem Building Chemicals, P.O. Box 40206, Lebanon (corresponding author). E-mail: jassaad@ndu.edu.lb 2 Associate Professor and Chair, Dept. of Civil Engineering, Notre Dame Univ., P.O. Box 72, Lebanon. E-mail: jharb@ndu.edu.lb Note. This manuscript was submitted on October 3, 2011; approved on June 28, 2012; published online on August 25, 2012. Discussion period open until October 1, 2013; separate discussions must be submitted for individual papers. This paper is part of the Journal of Materials in Civil Engineering, Vol. 25, No. 5, May 1, 2013. © ASCE, ISSN 0899-1561/ 2013/5-580-588/$25.00. The pressure may be induced by air or mechanical consolidation using a compression machine. For example, Bolton and McKinley (1997), Picandet et al. (2011), and Khayat et al. (2004) used air pressures in the range of 5.1–58.4, 10–100, and 0–700 kPa, respectively, to evaluate filtration properties of cement paste and concrete mixtures. Values of k in the order of 10−4 to 10−5 cm=s were derived from slurry mixtures made with various cement types and w=c ranging from 0.6 to 1 (Bolton and McKinley 1997). Khayat et al. (2004) found that the collected bleed water over a 10-min filtration period is dependent on mixture composition and can be directly related to permeability of fresh concrete deducted from Darcy’s law. Using the one-dimensional consolidation test, Uzomaka (1969) reported that plastic concrete behaves similarly to remolded clay soil of low compressibility. The derived k values were in the order of 10−8 cm=s and largely influenced by the mixture composition. Picandet et al. (2011) found that cement pastes with w=c varying from 0.3 to 0.4 behave according to the soil consolidation theory when tested using a displacement-controlled consolidometer. The authors found that hydration of cement does not result in noticeable decrease in permeability of tested mixtures during the first hour after mixing, and the k value is in the order of 10−5 to 10−6 cm=s. It is to be noted that the traditional approaches to evaluate k including the filtration and consolidation tests induce changes in the materials porous network due to applied pressure gradients (Picandet et al. 2011). This can result in higher effective stresses in the lower part of the tested samples together with a decrease in the void ratio due to forced consolidation and settlement. Objectives of the Research Project The notion of permeability has been mostly developed in soil mechanics to evaluate the ease with which fluid moves through the tortuous path of a solid skeleton with interconnected voids (Das 2010). Such measurement can be used for stability analyses of earth and retaining structures, and to estimate the quantity of underground seepage under various hydraulic conditions. The value 580 / JOURNAL OF MATERIALS IN CIVIL ENGINEERING © ASCE / MAY 2013 J. Mater. Civ. Eng. 2013.25:580-588. of k (cm=s) is basically deduced from the measured percolating flow rate (Q, cm3 =s) through a specimen section (S, cm2 ) from Darcy’s law as Q=S ¼ ki, where i denotes the vertical hydraulic gradient (dimensionless). Four empirical models developed by Hazen (1930), KozenyCarman (Kozeny 1927; Carman 1956), Amer and Awad (1974), and Chapuis (2004) to estimate permeability of soils are given in Eqs. (1)–(4), respectively. Downloaded from ascelibrary.org by UNIVERSITY OF PITTSBURGH on 08/01/13. Copyright ASCE. For personal use only; all rights reserved. kðcm=sÞ ¼ CH × D210 ð1Þ Eq. (1) is used for determining k in loose and clean sand, where CH is a coefficient varying from 1 to 1.5, and D10 (mm) is the particle size for which 10% of the soil is finer. 2 3 2 1 100% e kðcm=sÞ ¼ 1.99 × 104 × × P × SF ½fi =DðavÞi 1þe ð2Þ where e = void ratio, SF = shape factor varying from 6 to 8 depending on the angularity of the individual soil particles, fi = percent fraction of particles between two consecutive sieve sizes, and DðavÞi = average particle size between consecutive sieves. 3 e 2.32 kðcm=sÞ ¼ 35 × ð3Þ × C0.6 u × D10 1þe Eq. (3) is used for estimating k in granular soil, where D10 is in mm, e = void ratio, and Cu = coefficient of uniformity. e3 0.7825 kðcm=sÞ ¼ 2.462 × D210 × ð4Þ 1þe Eq. (4) is used for determining k in the range of 10−1 to 10 cm=s for natural uniform sand and gravel, but can be extended for natural silty sands without plasticity. Value of D10 is in mm and e = void ratio. During the dormant period of cement hydration, fresh mortars or concrete behave as weakly bonded materials submerged in fluid medium, and thus can be regarded as soil (Alexandridis and Gardner 1981; Assaad and Harb 2011). Therefore, the main objective of this paper is to evaluate suitability of the permeameter test to assess permeability of fresh mortars and concrete. Universally available in most research centers, the permeameter test is standardized [ASTM D2434 (ASTM 2006); ASTM D5084 (ASTM 2010b)] and quite simple to be realized, thus unifying the characterization of permeability. Parameters tested included cement content, w=c, coarse aggregate, and various concentrations of high-range water reducer (HRWR), silica fume, calcium stearate, and viscosity-modifying admixture (VMA). Validation and comparison of the investigated k values with theoretical models developed on soil are established. Such data are particularly useful for researchers, concrete engineers, and contractors to standardize testing protocols and optimize the hydromechanical properties of concrete. −3 Experimental Program Materials Portland cement and silica fume conforming to ASTM C150 Type I (ASTM 2012a) and ASTM C1240 (ASTM 2012b), respectively, were used in this project. The surface area of the cement (Blaine) and silica fume (BET) were 340 and 20,120 m2 =kg, respectively; and their specific gravities were 3.14 and 2.22, respectively. The cement had C3 S, C3 A, and Na2 Oeq . values of 60.4%, 6.6%, and 0.73%, respectively. Continuously graded ASTM C33 (ASTM 2011) crushed limestone aggregate with 20-mm nominal size and well-graded siliceous sand with 4.75-mm nominal size were used. The coarse aggregate and sand had fineness moduli of 6.4 and 2.5, respectively, and bulk specific gravities of 2.71 and 2.69, respectively. A polycarboxylate-based HRWR conforming to ASTM C494 (ASTM 2012c) Type F was used; its solid content and specific gravity were equal to 40% and 1.11, respectively. A powder welan gum VMA was used; it was diluted in 5% mixing water before adding to mortar or concrete. A calcium stearate product intended to impart water repellency and reduce efflorescence in cementitiousbased products was also used. It is a white powder compound of calcium with fine mixture of solid organic acids and some fatty acids obtained from edible sources, harmless to the environment, having a bulk density of 0.38. Finally, a sodium gluconate-based set-retarder was used to reduce workability loss during testing. Mixture Proportions As summarized in Table 1, four concrete series made with 300, 350, 400, and 450 kg=m3 of cement were investigated in this project. The sand-to-total aggregate ratio remained fixed at 0.46. The mortars were proportioned using the concrete-equivalent-mortar (CEM) approach, i.e., same concrete compositions except that the coarse aggregates were replaced by an equivalent quantity of sand to take into consideration the amount of water that can be absorbed onto their surfaces during mixing. More details on the method for proportioning CEM mixtures can be seen in Schwartzentruber and Catherine (2000) and Assaad et al. (2009a). In each series, different combinations of w=c (0.35–0.65), silica fume (0–10% of cement), calcium stearate (0–0.15% of cement), and VMA (0–0.08% of cement) were tested. Unless otherwise specified, the dosage of HRWR was adjusted to secure a concrete slump of 180 10 mm according to ASTM C143 (ASTM 2012d) or an equivalent CEM flow of 210 10 mm following five drops on the flow table according to ASTM C1437 (ASTM 2007; Assaad et al. 2009a). To minimize the effect of workability loss on permeability measurements during the first 30-min after mixing, the set-retarder was used at dosages of 0.6% and 0.4% of the cement weight in concrete and CEM mixtures, respectively. Table 1. Mixture Composition of Evaluated Concrete and CEM Series Series Series Series number 1 number 2 number 3 number 4 Type I cement (kg=m3 ) Silica fume (% of cement) w=c VMA (% of cement) Calcium stearate (% of cement) HRWR (% of cement) Concrete mixture Sand (0–4.75) (kg=m3 ) Coarse aggregate (4.75–20) (kg=m3 ) Vol. sand/Vol. cement paste Vol. coarse aggregate (L=m3 ) Sand/(sand+coarse aggregate) Corresponding CEM mixture Sand (0–4.75) (kg=m3 ) Vol. sand/Vol. cement paste 300 350 400 450 Varying from 0 to 10 Varying from 0.35 to 0.65 Varying from 0 to 0.08 Varying from 0 to 0.15 Various dosages to achieve different consistencies 960 1,120 930 1,080 890 1,040 840 980 1.58 418 0.46 1.36 401 0.46 1.14 386 0.46 0.96 364 0.46 1,150 1.83 1,060 1.56 1,005 1.29 940 1.07 JOURNAL OF MATERIALS IN CIVIL ENGINEERING © ASCE / MAY 2013 / 581 J. Mater. Civ. Eng. 2013.25:580-588. Downloaded from ascelibrary.org by UNIVERSITY OF PITTSBURGH on 08/01/13. Copyright ASCE. For personal use only; all rights reserved. Batching of Mixtures Water standpipe, Area a The mixing procedure for the concrete consisted of homogenizing the sand and coarse aggregate with half of the mixing water, then introducing the cementitious materials gradually over 30 s. The remaining part of water along with the HRWR, prehydrated VMA, calcium stearate, and set-retarder were then added and mixed for 1 min. After a rest period of 30 s, the concrete was remixed for 2 additional min. The same mixing procedure was adopted for the CEM, except that the coarse aggregates were removed from the batch. Testing and sampling of all concrete and CEM mixtures were made at room temperature of 23 2°C and 50% 5% relative humidity. It is to be noted that all mortar and concrete mixtures exhibited fresh air contents of 5.3% 0.8% and 2.3% 0.5%, respectively, which were determined according to ASTM C231/C231M (ASTM 2010a) test method. Inlet water valve L where a (cm2 ) = cross-sectional area of the inlet water valve (equal to 2.01 cm2 ), A (cm2 ) = cross-sectional area of specimen, h2 Specimen, Area A Datum Outflow Permeability Testing of Mortars and Concrete In general, permeability of soils is measured using a permeameter test following either the constant-head or falling-head method. The former method is recommended for coarse-grained soils where k is expected to be smaller than 10−5 cm=s, or when the soil contains 90% or more particles that are retained on the 75-μm sieve (Das 2010). Conversely, the falling-head test is suited for testing finegrained soils where the k value is expected to be within the range of 10−5 to 10−8 cm=s, or when the soil contains 10% or more particles passing the 75-μm sieve. Therefore, the falling-head method was selected in this study for testing mortar and concrete materials containing fine particles such as cement and silica fume. A commercially available soil permeameter apparatus was used for testing. Different steel-made cells having diameter/height dimensions of 102=105, 152=115, and 305=230 mm=mm were used for this purpose. Their inner surfaces were coated with a thin layer of specially made grease to reduce eventual water leakage along the sides of the cell (Engineers Manual 1110-2-1901 1986). To avoid entrapment of air, the tested material was well compacted using a tamping device in three layers of approximately similar heights. Two filter papers were placed between the upper and lower perforated plates and the tested material to retain approximately 96% of all particles greater than 1 μm. De-aired distilled water at room temperature was used during testing. This is essential to minimize the amount of air dissolved in water, which can collect fine bubbles at the solid particles/water interface and reduce permeability (Engineers Manual 1110-2-1901 1986). More details on the falling-head method determined on soils can be seen in various geotechnical books such as Das (2010). The permeameter stand consisted of a metal frame with water tank adjustable in height between 1,500 and 4,500 mm. This allows monitoring the extent of hydraulic gradient (i) applied on top of the tested specimen to values ranging from 10 to approximately 55. The value of i is being calculated as the ratio of total head of water under motion to the length of tested specimen. After opening the inlet water valve on top of the cell, outflow is observed to ensure a continuous flow regime (i.e., indicating complete saturation of the tested specimen) where water constantly trickles out from the outflow valve (Fig. 1). The time needed to reach such regime varied from 4 to 10 min, depending on mixture composition. After ensuring continuous flow, the value of k was determined as follows: a L h kðcm=sÞ ¼ × ð5Þ × ln 1 A Δt h2 h1 Cylinder Fig. 1. Sketch for the permeameter test, falling-head method L (cm) = height of specimen, and Δt (s) = time needed for the total head to drop from clearly marked graduations h1 to h2 (Fig. 1). Generally, Δt in the range of 2–8 min was obtained throughout testing to drop the level of water from h1 to h2 , again depending on the mixture composition. The maximum total time that was needed to prepare the mix (i.e., concrete or mortar), place in the cell, ensure a continuous flow regime, and testing permeability was less than approximately 25 min. Bleeding and Surface Settlement of Tested Mortars and Concrete In addition to permeability, bleeding and surface settlement responses of tested materials were evaluated. Bleeding was determined according to ASTM C232/C232M (ASTM 2009) test method, which involves measuring the relative quantity of mixing water that has bled from the freshly cast material in a container. The percent of bleeding water was obtained by dividing the collected water by the total mixing water in the tested mortar or concrete specimen. Settlement of fresh mortars was determined using a traditional oedometer apparatus commonly used for measuring onedimensional consolidation of clays and other compressible soils (Assaad and Harb 2011). Such test was found adequate to assess settlement of cementitious-based materials made with different compositions. The CEM sample having 71.4-mm diameter and 20-mm height was encased between fiber glass filters placed at its top and bottom surfaces. The displacements were recorded using a 0.002-mm dial gage after reaching a steady-state condition following the application of 2-kg normal load. As for the plastic concrete, surface settlement was determined using a polyvinyl chloride (PVC) column measuring 200 mm in diameter and 600 mm in height (Assaad et al. 2004). The settlement was monitored using a 0.002-mm dial gage fixed on top of a thin acrylic plate placed at the upper concrete surface until a steady-state condition is reached. Assaad and Harb (2011) reported that concrete settlements obtained from the PVC column can be well correlated to those determined on CEM using the oedometer test. 582 / JOURNAL OF MATERIALS IN CIVIL ENGINEERING © ASCE / MAY 2013 J. Mater. Civ. Eng. 2013.25:580-588. Effect of Hydration Time In order to determine the effect of hydration time on variations of permeability, the k values were measured at different elapsed times following initial mixing on several mortar and concrete mixtures. The hydraulic gradient was fixed at 25 2. The specimen remained in the permeameter cell during testing, and the inlet water valve opened to realize the measurement at specific time intervals, and then closed back again. In parallel, the setting time was determined on a separate specimen by penetration resistance according to ASTM C403/C403M (ASTM 2008) test method. Typical variations of k and penetration resistance obtained on CEM made with 350 kg=m3 cement and 0.5 w=c are plotted in Fig. 3. As expected, the k values gradually decreased as a function of time during the initial 200 min after mixing due to the loss in mixture’s consistency and continuous change in the pore network structure as the cement reacts with water. Beyond approximately 250 min, which roughly coincides with the mortar’s initial setting time, the k value sharply dropped toward zero. This result is in agreement with the findings of Garcia et al. (2008) who reported that initial setting time reflects a percolation threshold affecting connectivity between solid particles and voids within the newly hardened cement paste. 4 k × 10-5, cm/s Effect of Hydraulic Gradient (i) Permeability computed on the basis of Darcy’s law is limited to the condition of complete saturation of specimen and laminar flow characterized by straight and parallel flow lines (Engineers Manual 1110-2-1901 1986). Therefore, for example, for highly plastic clays of low permeability, Darcy’s law may not hold as the flow rate is so small and the soil considered being impervious. In contrast, at high i values, the flow becomes turbulent with fluctuations in fluid velocity in both parallel and transverse directions. This can result in significant changes in the specimen structure due to washing out of the finest particles and dissolution/precipitation of ions toward the bottom of the sample (leaching effect). To evaluate the validity of Darcy’s law, permeability measurements were conducted at different i values ranging from 10 to 55 on various mortar and concrete mixtures. As can be seen in Fig. 2, the variations in k due to different hydraulic gradients did not exceed 5% from the mean value, indicating that permeability is independent from i. Therefore, k of fresh mortars and concrete determined using the falling-head method can be regarded as valid when computed with respect to Darcy’s law. 20 Beginning of setting time Permeability 3 15 Setting time 2 10 Mortar with 350 kg/m³ cement and 0.5 w/c 1 5 Initial set at 3.5 MPa 0 0 50 100 150 200 Time, min 250 300 350 0 400 Fig. 3. Effect of hydration time on k and penetration resistance (cell of 102-mm diameter was used for testing at i ¼ 25 2) Effect of Specimen’s Volume Generally speaking, higher permeability values were measured when increasing the specimen’s volume. For example, as can be seen in Fig. 4, the k value increased from 4.9 to 5.1 and 8.3 × 10−5 cm=s for the CEM tested using the 102, 152, and 305 mm diameter cells, respectively. The increase in permeability was particularly important in concrete, as the k value has almost doubled when the cell diameter increased from 102 to 305 mm (Fig. 4). In geotechnical engineering, the increase in permeability when increasing sample’s volume is attributed to increased relative voids and hydraulic defects such as cracks, fissures, sand lenses, which have statistically bigger chance of being present in a large sample compared with a small one (Boynton and Daniel 1985). In fresh mortars and concrete, the increase in k may be related to an increase in the relative void ratio along with higher cement/sand/ aggregate surface interfaces present in the larger cell that can increase easiness of water percolation. Repeatability of Testing Several mortar and concrete mixtures made with different compositions were repeated five to seven times to evaluate repeatability of the falling-head method. The 102-mm diameter cell was used, and a constant hydraulic gradient of 30 3 was applied. The standard deviation among various measurements was found to range from 0.05 to 1.3 × 10−5 cm=s, with the resulting coefficient of variation (COV) varying from 1.3% to 6.5%. The COV is taken as the ratio between standard deviation and mean values, multiplied by 100. Compared with other testing methods, a COV less than 6.5% obtained from the permeameter test can be considered as quite acceptable. For instance, COV values of 8.1% and 12% were reported for the surface settlement determined on mortars using the oedometer 10 16 8 14 Mixtures with 350 kg/m³ cement content 6 4 2 0 CEM Concrete 12 k × 10-5, cm/s k × 10-5, cm/s Downloaded from ascelibrary.org by UNIVERSITY OF PITTSBURGH on 08/01/13. Copyright ASCE. For personal use only; all rights reserved. Phase I: Validity of the Falling-head Method to Assess Permeability of Fresh Mortars and Concrete 25 Penetration resistance, MPa 5 Test Results and Discussion Mortar: w/c = 0.55 Concrete: w/c = 0.55 Concrete: w/c = 0.4 Mortar: w/c = 0.4 10 8.8 8 6 14.5 Mixtures with 300 kg/m³ cement and 0.45 w/c 8.3 6.9 4.9 5.1 4 2 0 10 20 30 40 Hydraulic gradient (i ) value 50 60 Fig. 2. Effect of hydraulic gradient on k values (cells of 102- or 152-mm diameter were used for testing CEM or concrete, respectively) 0 102 / 105 152 / 115 305 / 230 Cell diameter / height dimensions, mm Fig. 4. Effect of sample dimensions on k values JOURNAL OF MATERIALS IN CIVIL ENGINEERING © ASCE / MAY 2013 / 583 J. Mater. Civ. Eng. 2013.25:580-588. The use of higher cement content resulted in decreased k (Fig. 6); a value of 1.6 × 10−5 cm=s was obtained for the mortar made with 450 kg=m3 cement and 0.5 w=c. This can be attributed to higher compaction rates which hinders water movement. Furthermore, mixtures containing higher cement contents require lower HRWR demand to achieve the needed flowability, which may increase cohesiveness (Assaad et al. 2004) and result in lower permeability. Effect of Silica Fume. The fine silica fume particles are known by their ability to improve compaction and reduce bleeding of freshly mixed mortars and concrete, thus leading to reduced permeability (Table 2). For example, k decreased from 1.6 to 0.85 × 10−5 cm=s for the CEM made with 450 kg=m3 cement and 0.5 w=c with the addition of 8% silica fume. Such decrease was from 3.1 to 1.6 × 10−5 cm=s for the equivalent concrete mixtures. test and on concrete using the 600-mm PVC column, respectively (Assaad and Harb 2011). Phase II: Permeability of Freshly Mixed Mortars and Concrete Effect of Mixture Composition on k Values Effect of Coarse Aggregates. Good relationship with high correlation coefficient (R2 ) of 0.95 is obtained between k values determined on CEM and those determined on concrete (Fig. 5). However, concrete incorporating coarse aggregates exhibited k of 40–120% greater than the one determined on mortar. Just like in soils where k is affected by the particle size (Das 2010), this indicates that water percolates easily in cementitious-based materials containing coarse aggregates. Effect of w=c and Cement Content. Typical variations of k for CEM made with various w=c and cement contents are illustrated in Fig. 6. Mixtures made with reduced w=c are shown to yield lower permeability. For example, k decreased from 8.6 to 4.9 × 10−5 cm=s for CEM prepared with 300 kg=m3 cement and w=c of either 0.65 or 0.45, respectively. In newly mixed cementitious materials, Picandet et al. (2011) reported that the void volume representing the degree of porosity through which water percolates can be assumed equal to the water volume, and thus expressed as a function of w=c. Therefore, mixtures prepared with lower w=c are expected to possess lower porosity that can slow down water percolation in the tested specimen. 14 k of concrete × 10-5, cm/s Downloaded from ascelibrary.org by UNIVERSITY OF PITTSBURGH on 08/01/13. Copyright ASCE. For personal use only; all rights reserved. More than 50 mixture combinations were tested in this project. Table 2 summarizes typical permeability, bleeding, and surface settlement responses obtained on CEM and concrete. Permeability cells of 102-mm or 152-mm diameter were used for testing CEM or concrete, respectively, at i values of 20 2. 12 y = 1.54 x R ² = 0.95 10 8 6 CEM tested in cell φ = 102 mm Concrete tested in cell φ = 152 mm i = 20 ± 2 0.05 < St. deviation < 1.21 x 10-5 cm/s 1.3% < COV < 6.5% 4 2 0 0 1 2 3 4 5 6 k of CEM × 10-5, cm/s 7 8 10 9 Fig. 5. Relationship between k determined on CEM and concrete mixtures Table 2. Typical Results of k, Surface Settlement, and Bleeding Determined on CEM and Concrete Mixtures Cement content (kg=m3 ) 300 350 400 450 Silica fume (% of cement) — — — — — — — — — — 7 — — — 4 — — 10 — — 2 — — 8 CEM properties Concrete properties w=c VMA (% of cement) Calcium stearate (% of cement) kðCEMÞ × 10−5 (cm=s) SettleðCEMÞ (mm) BleedðCEMÞ (%) kðConcÞ × 10−5 (cm=s) SettleðConcÞ (mm) BleedðConcÞ (%) 0.45 0.45 0.45 0.52 0.52 0.65 0.4 0.4 0.55 0.55 0.55 0.55 0.42 0.46 0.46 0.46 0.51 0.51 0.35 0.35 0.35 0.5 0.5 0.5 — 0.03 — — 0.05 — — 0.015 — 0.06 — — 0.01 — — 0.05 — — — 0.02 — — 0.08 — — — 0.1 — — — — — — 0.05 — 0.12 — — — — — 0.08 — 0.05 — — — — 4.9 2 4.8 6.2 5 8.6 3.8 2.7 5 1.9 3.6 3.9 2.1 3.3 2.8 1.7 4.2 1 0.9 0.045 0.74 1.6 0.28 0.85 1.39 1.24 1.62 2.54 1.84 3.2 1.55 1.32 2.15 1.51 2.06 1.82 1.12 1.5 1.37 1.28 1.88 0.75 0.45 0.27 0.85 1.4 0.42 1.03 3.9 3.4 3.58 4.26 2.85 5.15 2.2 1.74 3.82 2.6 3.5 3.26 1.44 2.3 1.98 1.24 2.66 0.98 1.42 0.41 1.29 1.15 0.76 1.12 6.9 — — 8.8 — 12.5 5.4 — 8.2 2.6 — 7.1 — 6.1 5.4 3.7 — 1.8 2 — — 3.1 0.63 1.6 — — — 2.52 — 4.14 2.28 — 3.72 2.46 — 3.18 — 1.7 1.62 1.21 — — — — — 1.56 0.66 1.08 — — — 7.2 — 8.4 5.1 — 7.5 6.2 — 6.4 — 4.4 3.1 3.4 — — — — — 2.5 1.8 2.3 Note: Permeability cells of 102- or 152-mm diameter were used for testing CEM or concrete, respectively, at i values of 20 2. The COV for kðCEMÞ and kðConcÞ is less than 6.5%. HRWR is adjusted to achieve concrete slump of 180 10 mm and CEM flow of 210 10 mm. Fixed dosages of set-retarder of 0.6% or 0.4% of cement weight were used in concrete and CEM mixtures, respectively. 584 / JOURNAL OF MATERIALS IN CIVIL ENGINEERING © ASCE / MAY 2013 J. Mater. Civ. Eng. 2013.25:580-588. 10 CEM mixtures (COV < 3.3%) 8.6 k × 10-5, cm/s 8 6.2 6 5 4.9 4.2 4 1.6 0 Cement, kg/m³ w/c 300 300 300 350 400 450 0.45 0.52 0.65 0.55 0.51 0.5 Fig. 6. Effect of cement content and w=c on k values (cell of 102-mm diameter was used for testing at i ¼ 20 2) Effect of VMA. All CEM and concrete incorporating VMA exhibited a decrease in k, particularly when such agent is added at high concentration (Table 2). For example, the k value decreased from 1.6 to 0.28 × 10−5 cm=s when the VMA was added at 0.08% of cement weight in the mortar made with 450 kg=m3 and 0.5 w=c. This can be attributed to the mode of function of the VMA that binds part of the water (either mixing water or the one being circulated from the falling-head method), thus improving the overall thixotropy and stability of the mixture (Assaad et al. 2004). Effect of Calcium Stearate. The addition of calcium stearate led to reduced permeability levels in the tested mixtures (Table 2); a decrease from 5 to 3.9 × 10−5 cm=s was noted when the calcium stearate was incorporated at 0.12% of cement weight in the CEM prepared with 350 kg=m3 cement and 0.55 w=c. Such decrease was from 8.2 to 7.1 × 10−5 cm=s in the corresponding concrete mixtures. This can be related to the fact that the calcium stearate imparts water repellency when added to cementitious-based materials, thus interfering with the free movement of water in the specimen. Effect of Consistency. Typical variations of k determined on mixtures possessing different levels of consistency obtained by adjusting the dosage of HRWR are plotted in Fig. 7. Clearly, a considerable increase in k was obtained for mixtures having higher consistency levels, mainly due to a decrease in the mixture’s cohesiveness and stability that allow water to permeate easily in the matrix. For example, such increase was from 3.7 to 12.8 × 10−5 cm=s when concrete slump increased from 140 to 245 mm, respectively. 12.8 Determination of the Void Ratio, e The determination of the void ratio is based on a study carried out by Picandet et al. (2011) to assess permeability of fresh cementitious materials using an oedometer compression test. Such materials are considered fully saturated after mixing, and thus the void CEM (COV < 3.3%) 6.1 6 3.7 5.7 3.3 2.4 1.12 2 140 180 210 245 Concrete slump, mm 130 Bleeding, % Surface settlement, mm 5 8.5 8 0 Mixtures with 400 kg/m³ cement and 0.46 w/c Concrete (COV < 5.4%) 10 4 An attempt was made to evaluate applicability of empirical soil models described earlier in Eqs. (1)–(4) to predict permeability of fresh mortars. Twelve mixtures made with different w=c, cement, and silica fume contents were tested using the 102-mm diameter cell. The determination of the various parameters used in Eqs. (1)–(4) including e, D10 , D60 , and Cu is presented in the following sections. It is to be noted that the powder VMA or calcium stearate was not added to the tested mortars, given that their percentages are quite small to be detected by the mixture particle-size distribution curves (i.e., D10 and D60 ) whereas their effects on permeability are highly significant. CEM properties 12 Phase III: Use of Empirical Soil Models to Estimate Permeability of Fresh Mortars 6 14 k × 10-5, cm/s Downloaded from ascelibrary.org by UNIVERSITY OF PITTSBURGH on 08/01/13. Copyright ASCE. For personal use only; all rights reserved. 2 Validation of k Using Bleeding and Surface Settlement Responses The bleeding and surface settlement properties determined either on mortar or concrete mixtures are well related within each other (R2 > 0.7). The bleeding phenomenon reflects the upward migration of interstitial solution toward the upper material’s surface (Josserand et al. 2006). It is normally coupled with a higher level of consolidation, which would lead to greater surface settlement (Assaad et al. 2004). Generally, the increase in cement content, decrease in w=c, and incorporation of silica fume, VMA, or calcium stearate were found to reduce bleeding and surface settlement responses (Table 2). Additional discussion regarding the effect of mixture composition on such parameters can be seen in Assaad et al. (2004) and Khayat et al. (2004). The relationships between bleeding measured according to ASTM C232/C232M (ASTM 2009), surface settlement determined using the one-dimensional oedometer test, and k values determined using the falling-head method on CEM mixtures are plotted in Fig. 8. As can be seen, the increase in k value is associated with an increase in bleeding and surface settlement with R2 greater than 0.82. Similar relationships were obtained among such properties determined on concrete, with R2 greater than 0.71. This suggests that the k value determined using falling-head method constitutes a suitable index to reflect hydromechanical properties (including bleeding and surface settlement) of freshly mixed mortars and concrete. y = 0.55 x + 0.73 R ² = 0.82 4 3 2 y = 0.29 x + 0.55 R ² = 0.85 1 175 210 0 240 0 CEM flow, mm Fig. 7. Effect of consistency on k values (cells of 102- or 152-mm diameter were used for testing CEM or concrete, respectively, at i ¼ 20 2) 1 2 3 4 5 6 k of CEM × 10-5, cm/s 7 8 9 10 Fig. 8. Relationships between k determined on CEM with respect to bleeding according to ASTM C232/C232M (ASTM 2009) and surface settlement (oedometer test) JOURNAL OF MATERIALS IN CIVIL ENGINEERING © ASCE / MAY 2013 / 585 J. Mater. Civ. Eng. 2013.25:580-588. Table 3. Values of e, D10 , D60 , Cu , and k Calculated Using Different Empirical Soil Models Cement content (kg=m3 ) 300 350 450 w=c 0 18 0 35 0 0 0 0 45 0 0 0 0.35 0.4 0.65 0.35 0.45 0.65 0.35 0.65 0.35 0.35 0.5 0.65 e D10 (mm) D60 (mm) 0.301 0.315 0.575 0.303 0.425 0.607 0.340 0.624 0.317 0.341 0.546 0.684 0.052 0.05 0.052 0.047 0.048 0.048 0.045 0.045 0.038 0.04 0.04 0.04 0.19 0.18 0.19 0.16 0.18 0.18 0.14 0.14 0.12 0.13 0.13 0.13 Cu Eq. (1) Hazen Eq. (2) Kozeny-Carman Eq. (3) Amer and Awad Eq. (4) Chapuis Actual k obtained by testing × 10−5 (cm=s) 3.65 3.60 3.65 3.40 3.75 3.75 3.11 3.11 3.16 3.25 3.25 3.25 270 250 270 221 230 230 203 203 144 160 160 160 104 94.8 319 71.2 157 406 59.2 343 16.2 78.6 213 266 168 172 965 129 364 938 153 775 85.3 120 428 772 117 122 460 101 216 454 122 434 79.9 102 275 436 3.9 3.45 8.6 1.9 4.15 6.7 0.98 5.1 0.22 0.9 1.6 3.96 Note: In Eq. (1), the Hazen’s constant (CH ) is taken to be equal to 1. In Eq. (2), the shape factor (SF) is taken to be equal to 7.5. e¼ W γs S γw ð6Þ During oedometer testing, the mortar’s height (h) is always lower than its initial height (h0 ) due to consolidation, which squeezes out part of the mixing water initially contained in the material. Assuming that the dry solid mass of the specimen (S) is constant (i.e., only the fluid phase can flow through the filter cake), a variation Δh in the mortar’s initial height induces W=S variation with a corresponding void ratio variation (Δe) as follows: Δh Δe ¼ e − e0 ¼ ð1 þ e0 Þ h0 ð7Þ Hence, for example, to determine Δe in the mortar made with 300 kg=m3 cement and 0.65 w=c, the actual 3.2-mm settlement measured using the oedometer (Table 2) is divided by the mortar’s initial height of 20 mm, and the result multiplied by (1 þ e0 ). The e values obtained in this study varied from approximately 0.3 to 0.7 (Table 3); note that typical e values reported in the literature for loose or dense sand and silty sand are in the range of 0.4–0.8 (Das 2010). Determination of D10 , D60 , and Cu of Dry Mortars The particle-size distribution curves for the various combinations of tested materials were determined by ordinary sieve analysis. The sand was oven-dried before use, and then mixed with the cement and silica fume according to the ratios given in Table 1. Typical gradation for the dry mortar made with 300 kg=m3 cement is plotted in Fig. 9, along with the determination of D10 , D60 , and Cu . The results obtained for tested dry mortars are given in Table 3. Calculated k Using Empirical Soil Models versus Determined k by Testing The determined e, D10 , D60 , Cu , and particle-size distribution are used to calculate four kinds of k according to Eqs. (1)–(4) (Table 3). Similar k values were abnormally obtained when applying Hazen’s empirical model [Eq. (1)] on mortars prepared with a given cement content but different w=c, and consequently different e values. For example, a value of 270 × 10−5 cm=s was obtained for the mix made with 300 kg=m3 cement despite the change in w=c from 0.35 to 0.65 (Table 3). This indicates that Hazen’s model is of limited use and thus is not adapted to estimate permeability of cementitious materials as it does not take the w=c into consideration. The relationships between calculated k values using Eqs. (2)–(4) with respect to those determined by testing using the permeameter cell are plotted in Fig. 10 (the relationships were forced to intercept the graph’s origin). On average, the calculated k was 48–120 times greater than the actual k determined by testing. This can be related to the fact that the empirical equations were originally developed 100 D10 = 0.052 mm Passing percentage (by mass) volume (i.e., void-to-solid volume ratio) can be assumed equal to the water or liquid volume. It can be written as a function of the water-to-solid mass ratio (W=S) and the specific unit weights of the solids (γ s ) and water (γ w ) as follows: Dry mortar with 300 kg/m³ cement D60 = 0.19 mm 80 Cu = D60 / D10 = 3.65 60 40 Natural sand Portland cement 20 0 0.001 0.01 D10 0.1 D60 Sieve size (mm) 1 10 Fig. 9. Typical determination of D10 , D60 , and Cu for dry mortar made with 300 kg=m3 cement 1.2×10-2 Calculated k using models, cm/s Downloaded from ascelibrary.org by UNIVERSITY OF PITTSBURGH on 08/01/13. Copyright ASCE. For personal use only; all rights reserved. 400 k calculated by models × 10−5 (cm=s) Silica fume (kg=m3 ) Eq. (3): y = 120 x R ² = 0.72 Eq. (2): Kozeny–Carman 1.0×10-2 8.0×10-3 Eq. (3): Amer and Awad Eq. (4): Chapuis Eq. (4): y = 63.8 x R ² = 0.56 6.0×10-3 4.0×10-3 2.0×10-3 0.0×100 0×100 Eq. (2): y = 48.2 x R ² = 0.65 2×10-5 4×10-5 6×10-5 8×10-5 Actual k determined by testing, cm/s 1×10-4 Fig. 10. Relationships between actual k determined by testing with respect to those calculated using different empirical soil models 586 / JOURNAL OF MATERIALS IN CIVIL ENGINEERING © ASCE / MAY 2013 J. Mater. Civ. Eng. 2013.25:580-588. 0.8 Commonly used empirical models in soil mechanics were found useful to predict permeability of fresh mortars made with different w=c and contents of cement or silica fume. However, the calculated k was 48–120 times greater than the actual k determined by testing. The model proposed by Amer and Awad yielded the best linear fitting with respect to actual k determined by testing, followed by the Kozeny-Carman and Chapuis models. Linear relationships were obtained between void ratio and logarithm of calculated k values. Eq. (2): Kozeny–Carman Void ratio, e 0.7 0.6 Eq. (3): Amer and Awad Eq. (4): Chapuis 0.5 0.4 R ² > 0.86 0.3 Downloaded from ascelibrary.org by UNIVERSITY OF PITTSBURGH on 08/01/13. Copyright ASCE. For personal use only; all rights reserved. 0.2 1×10–4 1×10–3 Logarithm of k, cm/s 1×10–2 Fig. 11. Relationships between mortars void ratios and logarithm of k calculated using different empirical soil models Acknowledgments The authors wish to acknowledge the financial support of the National Council for Scientific Research (CNRS), Lebanon. References for soil where no or little chemical activity occurs in presence of moisture. In case of mortars, hydration reactions take place as soon as the cement particles are in contact with water to form a semirigid, interlocking, and polycrystalline solid network that can slow down the rate of water percolation and reduce permeability (Bolton and McKinley 1997). Keeping in mind the differences in chemical nature between soil and mortar, the correlations plotted in Fig. 10 between calculated and actual k values can be considered as acceptable. The highest R2 of 0.72 resulted from Amer and Awad empirical model [Eq. (3)], suggesting that e, D10 , and Cu parameters present in this model are all relevant to properly estimate permeability of fresh mortars. The Kozeny-Carman model [Eq. (2)], which takes into consideration the fraction of particles between two consecutive sieve sizes and e yielded a moderate R2 of 0.65. The decrease in R2 to 0.56 with Eq. (4) (Chapuis) may be related to the fact that this model was developed for uniform sand and gravel with expected k in the range of 10−1 to 10−3 cm=s. In soil mechanics, it is common to observe linear relationships between void ratio and logarithm of k (Das 2010). Such observations are confirmed when plotting e versus log of calculated k using empirical models for the tested mortars (Fig. 11). High R2 exceeding 0.86 are obtained, indicating applicability of soil permeability theories and concepts to freshly mixed mortars. Summary and Conclusions The falling-head method realized using a soil permeameter is suitable to assess permeability of freshly mixed mortars and concrete. This method is independent of the hydraulic gradient (i), thus making valid the computation of k using Darcy’s law. Permeability measurements gradually decreased as a function of time after mixing until the mixture reaches initial setting, whereby k dropped sharply toward zero. Higher permeability values were obtained when increasing specimen’s volume. Permeability of fresh mortars and concrete is directly affected by the mixture composition. For example, mixtures prepared with higher cement content, lower w=c, lower consistency, and increased concentrations of silica fume, VMA, and calcium stearate were found to reduce k. Concrete incorporating coarse aggregates exhibited k values 40–120% greater than those determined on CEM, indicating that permeability increases with the increase in particle size. 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