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Effects of Mixing Variables on Early-Age Characteristics of

Portland Cement Systems


David Trejo, Ph.D., P.E., M.ASCE 1; and Lapyote Prasittisopin, Ph.D. 2

Abstract: The performance and economy of infrastructure system is dependent on the specifications used to construct it. Good specifications
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contain requirements that correlate with improved performance and/or economy. There are several standards and specifications for mixing
field concrete. These documents provide requirements for the mixing process. However, limited research has been performed on how mixing
time and number of drum revolutions affect concrete characteristics. With advanced technologies that can delay the set and improve the
workability, the current documents may not be applicable. This paper presents an assessment of pastes and mortars mixed for different times
and varying number of mixer revolutions. Early-age characteristics include the assessment of time-variant ion concentration in solution,
flowability, setting time, and chemical shrinkage. Results indicate that these early-age characteristics of pastes and mortars mixed in
the laboratory are influenced by the mixing time and number of mixer revolutions. The rate of dissolution (Rd ) of ions in solution and
temperature are the material parameters directly affected by the mixing processes and these parameters can alter the rates of hydration
reactions, resulting in changes of the early-age characteristics of cement systems. DOI: 10.1061/(ASCE)MT.1943-5533.0001610.
© 2016 American Society of Civil Engineers.
Author keywords: Mixing time; Number of mixer revolutions; Early-age characteristics; Ion concentration; Flowability; Setting time;
Chemical shrinkage.

Introduction performance. To better correlate specification values with the


concrete performance, the influence of mixing variables on the
The performance and economy of an infrastructure system are performance of cementitious systems should be performed to better
highly dependent on the standard specifications used to construct understand if value is being added. This research presents results
it. Specifications that place limits on materials, suppliers, and/or from a research program to evaluate the effects of the laboratory
contractors may result in increased construction and life cycle mixing processes on the early-age characteristics of portland
costs, especially if these specifications do not result in improved cement (PC) paste and mortar system. Research was performed
economy, constructability, or concrete performance. Historically on the hardened characteristics of pastes and mortars and on
prescriptive specifications should be switched to performance- concrete systems and results were shown (Prasittisopin and Trejo
based specifications so as not to limit the development of alterna- 2014). Results indicated increased mixing time and revolution can
tive materials and construction practices (Hooton 2008). These result in higher early-age strengths, but lower later-age strengths. If
specifications include the standard specifications and guidelines other materials (e.g., fly ash) are added, the systems will be more
for ready-mixed concrete. complex, leaving more questions. For instance, the effects of
Standard specifications and guidelines for ready-mixed concrete mixing time and number of revolutions of fly ash system were
specially for truck mixers, including ACI 304R (ACI 2000), ASTM studied by Prasittisopin and Trejo (2013) and the results showed
C94/C94M (ASTM 2012b), and AASHTO M157 (AASHTO that increased replacement level of fly ash can delay the hydration
2006), place limits on the mixing time at 90 min, maximum reactions and their compressive strengths do not apparently de-
concrete temperature at 28–38°C (75–100°F ), and/or total number crease. Therefore, the work in this study was conducted only for
of truck drum revolutions at 300 counts. Furthermore, 48 state plain PC, which provides better comprehension in their effects.
highway agencies (SHAs) limit the mixing time; 45 SHAs limit Better understanding of how mixing variables influence mixture
the concrete placement temperature; and 30 SHAs limit the total performance is needed to ensure existing specifications do actually
number of drum revolutions. These limits are in place because it add value. This study presents results from a laboratory evaluation
is believed that mixing variables can influence the early-age and of the early-age characteristics of PC paste and mortar systems
later-age performance characteristics of concrete products. subjected to different mixing times and different numbers of mixer
However, limited research has been performed to assess the influ- revolutions. The early-age characteristics assessed include the time-
ence of mixing time and number of drum revolutions on concrete variant concentration of ions in solution, flowability, setting time,
and chemical shrinkage.
1
Professor and Hal D. Pritchett Endowed Chair, School of Civil and
Construction Engineering, Oregon State Univ., Corvallis, OR 97333.
2
Researcher, Siam Cement Group, Building and Construction
Materials, Saraburi 18260, Thailand (corresponding author). E-mail: Background of Laboratory Mixing Process
lapyotep@scg.co.th
Note. This manuscript was submitted on March 3, 2015; approved on The concrete mixing process has been defined as the production
February 4, 2016; published online on April 22, 2016. Discussion period method required for the complete blending to produce a homo-
open until September 22, 2016; separate discussions must be submitted for geneous concrete (Mindess et al. 2002). The mixing process has
individual papers. This paper is part of the Journal of Materials in Civil been reported to influence the homogeneity and uniformity of con-
Engineering, © ASCE, ISSN 0899-1561. crete (Roy and Idorn 1993; Ferraris 2001; Rupnow et al. 2007).

© ASCE 04016094-1 J. Mater. Civ. Eng.

J. Mater. Civ. Eng., 04016094


In fact, Rupnow et al. (2007) reported that the mixing process from Lowke and Schiessl 2007): (1) the loading period (defined
might influence the cement hydration and the interfacial transition as the period when the mixing begins); (2) the mixing period
zone (ITZ) between aggregates and cement paste. Roy and Idorn (defined as the period after mixing initiates up to some optimum
(1993) also reported that although the dispersion mechanism mixing time); and (3) the extended-mixing period (defined as the
(mixing) of constituent particles in concrete was related to cement time after the optimum mixing time).
hydration, the quantification between mixing and hydration is The loading period is the period when the constituent particles
needed. Ferraris (2001) reported that the relationship between (the UCP and water) are introduced using external energy from a
the mixing process and macroscopic properties has not been clari- mixing apparatus. This typically occurs at lower shear rates. As the
fied. The vagueness in how the mixing limits affect homogeneity external energy is applied to the mixture, particles become more
and performance requires further investigation. distributed. After the loading period is finished, the process moves
In addition, Charonnat and Beitzel (1997) studied the mixing of into the mixing period. In this period, the degree of dispersion in-
concrete and reported that (1) filling time, (2) mixing time, and creases while the mixture is mixed at higher energies and higher
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(3) discharge time can all influence homogeneity and uniformity shear rates. The degree of dispersion gradually increases to some
of concrete mixtures. The authors also reported that fresh concrete maximum level within some reasonable time. Once (and if) the
mixtures that were discharged too fast resulted in segregation due to maximum level is achieved, the ultimate homogeneity of the fresh
excess mass flow energy. In addition, the degree of homogeneity mixture is achieved, resulting in maximum flowability and/or
and uniformity of concrete mixtures is reported to be dependent on workability. Mixing is likely to not improve the flowability after
mixture proportions, constituent material type and characteristics, maximum dispersion is achieved. This is because the particles
velocity of the mixing tool, geometry of the mixer, and material and are uniformly dispersed and capillary forces between water
environmental conditions during mixing (Ferraris 2001). The molecules and the surfaces and micropores are reduced to some
following sections provide background on the mechanisms of mix- minimum value. However, if maximum dispersion is not achieved
ing and how these mechanisms affect homogeneity and possibly within the initial mixing period, an extended mixing period can be
early-age and later-age characteristics of mixtures. beneficial. The summary of the relationship between dispersion and
deformation mechanisms of the mixing process is shown in Fig. 1.
Deformation Mechanisms of Mixing Process The extended-mixing period can result in decreased dispersion
and flowability (as shown in Fig. 1). It is believed that, as the con-
When water is first introduced to unhydrated cement particles vective deformation progresses, the cement particles become
(UCP) and the mixing process begins, two types of deformations smaller and debris particles (in the case of mortar and concrete)
occur between the water and the UCP. Fluid deformation from the are generated due to impact and abrasion forces between the mixing
constituent materials, referred to as a dispersive transport, occurs apparatus and the constituent particles. This has been reported to
first and continues throughout the mixing process. This is typically result in a change of concrete microstructures and performance
associated with Brownian motion and no energy inputs. When characteristics for self-consolidating concrete (SCC) (Takada
mixing begins, mechanical deformation occurs, which is also 2004). Diamond (2005) reported that a change of concrete
referred to as a convective transport. Both transport types have been
microstructure was observed when concrete mixtures were mixed
reported to influence the homogeneity of the mixtures (Lowke and
for longer periods (e.g., mixed for 90 min).
Schiessl 2007).
Several research programs have reported that mixing influences
The dispersive transport is a deformation process where individ-
the homogeneity of the mixture. However, how this homogeneity
ual particles (or smaller groups of particles) randomly collide. It is
influences mixture properties and characteristics has not been
believed that these collisions only occur over relatively short
well-documented. More research is needed to better understand
distances, as no external forces are typically involved. Therefore,
a potential impact of mixing time and number of mixer revolutions
the dispersive transport results in some dispersion of the cement
on the performance of cementitious systems.
particles over shorter distance, but does not uniformly distribute
these particles over larger volumes. However, this dispersive
transport is believed to have a significant effect on the homogeneity
of mixtures because it results in a significant increase of contact lower shear rates higher shear rates
areas between the cement particles and the water molecules. This
promotes localized homogeneous deformation, facilitates faster nu-
cleation process, and improves a void coalescence (Lowke and
Schiessl 2007). After water is introduced to the UCP, capillary
forces between water molecules and the surfaces and micropores
of constituent particles are created. These capillary forces result
in surface tension within the water, and consequently make parts
of water unable to disperse uniformly.
The convective transport is a forced, directed deformation. This
deformation typically occurs over a larger distance because external
energy is often being applied. The external energy from the mixing
apparatus disperses constituent particles within the mixer. Lowke
and Schiessl (2007) reported that the convective transport has less
Ion dispersion Loading Mixing Extended-mixing
influence on the dispersion of the UCP than the dispersive trans-
Convective transport
port. This is because during the dispersive transport individual UCP
can disperse, leading to higher contact areas between the UCP and Dispersive transport
the water, but during the convective transport the larger groups of
Fig. 1. Relationship between dispersion of particles and mixing
the UCP only move, resulting in fewer contact areas. The convec-
mechanisms
tive transport can be divided into three distinct periods (adapted

© ASCE 04016094-2 J. Mater. Civ. Eng.

J. Mater. Civ. Eng., 04016094


Correlation of the Laboratory and the Field Study Table 2. Mixing Conditions for Cement Pastes and Mortars

Correlation between many characteristics of paste, mortar, and con- First stage Second stage
crete mixed in the laboratory and in the field is lacking. Rupnow Mix Time Speed Time Speed Number of
et al. (2007) studied the two-step mixing process for cement paste, number (min) (rpm) (min) (rpm) mixing revolution
laboratory concrete, and field concrete mixing and reported that Paste
there was good correlation for concrete strength, slump, and air P1 0.5 140 1 140 210
content between the laboratory and field mixed concretes. Saucier P2 0.5 140 1 285 355
et al. (1990) investigated the air-void stability of lab mixed and P3 0.5 140 14 140 2,030
ready-mixed concrete with superplasticizer admixtures. The results P4 0.5 140 14 285 4,060
also showed a good correlation of the air-void distribution between P5 0.5 140 59 140 8,330
these two systems. However, no correlation was reported with other P6 0.5 140 59 285 16,885
early-age and later-age (mechanical and durability) characteristics. Mortar
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Because the correlation between lab and field mixed concrete is M1 1 140 1.5 140 280
M2 1 140 1.5 285 498
lacking, this paper presents the first work to better define the
M3 1 140 14.5 140 2,100
relationship between laboratory and field mixed concrete (pre- M4 1 140 14.5 285 4,203
sented in the future work). Specifically, this paper will provide a M5 1 140 59.5 140 8,400
laboratory assessment of PC pastes and mortars subjected to differ- M6 1 140 59.5 285 17,028
ent mixing regimes (time and mixer revolutions). It is anticipated
that this research will provide basic knowledge on the influence of
mixing variables and that the information can then be used to better and mortars evaluated in this study. Three mixing times (2, 15,
estimate the influence of mixing variables on concrete mixed in the and 60 min) and two mixing speeds (140 and 285 rpm) were evalu-
field. Hardened characteristics for PC systems were reported in ated. This resulted in 210; 355; 2,100; 4,060; 8,330; and 16,885
Prasittisopin and Trejo (2014). mixer revolutions for paste mixing and 280; 568; 2,170; 4,273;
8,470; and 17,098 mixer revolutions for mortar mixing. Note that
the control mixtures are identified as Mixture No. P2 and M2
Experimental Investigation
(mixing at 140 rpm for 0.5=1.0 min followed by mixing at 285 rpm
for 1.0=1.5 min). Triplicate specimens were assessed for all tests in
Materials this study.
Type I/II PC meeting requirements of ASTM C150 (ASTM 2012a) During hydration, the concentrations of ions in solution contin-
was used for all mixtures in this study. The chemical composition uously change. The hydroxyl (OH) ion concentration and related
and ASTM requirements for the cement are shown in Table 1. solution pH are important parameters that can influence the early-
Graded sand meeting ASTM C778 (ASTM 2013) was used for test- age characteristics and long-term performance of hydrated prod-
ing the flowability. ASTM D1193 (ASTM 2011) type II de-ionized ucts. As a result, this study assesses the concentration of OH ions
(DI) water [1 MΩ · cm (0.4 MΩ · in:) at 25°C (77°F)] was used for in solution at early ages. The OH ion concentration was evaluated
all mixtures and experiments. using a pH electrode. The water-cement ratio (w/c) of the cement
solutions for the OH ion concentration study was 4.0. Mixing for all
systems was performed using a magnetic stirrer rotating at 0, 400,
Methods and 800 rpm throughout the test. These rotations were selected
The mixing procedures for the cement pastes and mortars using a because the resultant ion concentrations are distinguishable. Note
laboratory mixer followed ASTM C305 (ASTM 2014). This that for the mixtures mixed at 0 rpm, the solutions were first mixed
standard provides guidelines for mixing cement pastes and mortars at 400 rpm for 3 min and then mixing was stopped. The mixing of
and includes two consecutive mixing stages: a low speed mixing the first step allows the UCP to be mixed with water before assess-
(140 rpm) in the first stage followed by an intermediate speed ing the influence of the mixing process. The time elapsed after
mixing (285 rpm) in the second stage. This evaluation included introducing the UCP to the solution is referred to here as the
adjusting the mixing time and mixing speed of the second stage hydration time. Solutions used for evaluating OH ions were
only. Table 2 shows the mixing conditions for the cement pastes analyzed at 5, 10, 15, 30, 45, 60, 90, 120, 150, 180, 210, and
240 min (and mixed at 0, 400, and 800 rpm).
The rates at which calcium (Ca), aluminate (Al), and silicate (Si)
Table 1. Chemical Composition and Requirements Meeting ASTM C150 ions dissolve and precipitate from the PC are also believed to in-
of PC (Data from ASTM 2012a) fluence the early-age characteristics. Therefore, to better under-
Composition Specification limit Percentage
stand the early-age characteristics of PC systems, concentrations
of Al and Ca ions in PC solutions were determined in this study.
SiO2 — 20.30 Silicate concentrations were not assessed because of equipment
Al2 O3 6.0 maximum 4.80
limitations.
Fe2 O3 6.0 maximum 3.50
MgO 6.0 maximum 0.70
The concentrations of Al and Ca ions were determined using
SO3 3.0 maximum 2.80 flame atomic absorption spectroscopy (FAAS). The mixing process
CaO — 63.9 for the Al and Ca ion concentration studies was similar to the
Loss on ignition 3.0 maximum 2.60 mixing process for OH ion concentration study. Ion concentrations
Insoluble residue 0.75 maximum 0.11 were determined at the same hydration times as the OH ion
CO2 — 1.80 concentration tests, with additional tests performed at 300, 360,
Limestone 5.0 maximum 3.20 and 420 min.
CaCO3 in limestone 70 minimum 97.80 At each hydration time, cement solution was decanted from the
Naeq 0.6 maximum 0.54
mixing container and then filtered using a vacuum pump and

© ASCE 04016094-3 J. Mater. Civ. Eng.

J. Mater. Civ. Eng., 04016094


No. 40 filter paper. Filtered solution was used for analyzing Al Average concentation of ions ðmmol=lÞ
RX ðmmol=l=minÞ ¼ ð1Þ
[10 mL (0.338 fl oz)] and Ca [1 mL (0.033 fl oz)] ion concentra- Hydration time ðminÞ
tions, respectively. Because high concentration of Ca ions in sol-
ution occurs at early ages, filtered solutions for analyzing Ca ion where x = either d for dissolution or p for precipitation.
concentration was diluted prior to the FAAS analyses. Extracted In addition to the ion concentration studies, the flowability of
and filtered solution for analyzing Ca ion concentration was diluted fresh mortars, setting time, and chemical shrinkage of the pastes
with 9 mL (0.297 fl oz) of DI water to obtain the solution within the were determined.
detection range of the FAAS. After filtering and/or diluting, 1 mL The flowability was determined following ASTM C1437
(0.033 fl oz) of lanthanum acid solution 50 g=L (0.42 lb=gal:) (ASTM 2007). The mortar specimens for the flowability test
lanthanum oxide (La2 O3 ) in 3M hydrochloric acid (HCl) was included mortars with w/c values of 0.4 and 0.485 and the
added to the solution. Concentration of Al ions was determined cement–fine aggregate ratio was 1∶2.75, as recommended in the
using the FAAS with nitrous oxide–acetylene gas at a wavelength standard for mixing mortars. Different w/c values of mortars were
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of 309.3 nm (1.22 × 10−5 in:) ignited at a temperature of 2,600– observed to determine. The setting times of all systems were
2,800°C (4,712–5,072°F). The Ca ion concentration was deter- determined following ASTM C191 (ASTM 2004). The w/c values
mined using FAAS with air–acetylene gas at a wavelength were 0.3 and 0.4. Temperatures of the pastes were measured
of 422.7 nm (1.66 × 10−5 in:) ignited at the temperature of immediately after mixing using an infrared thermometer. The
2,100–2,400°C (3,812–4,352°F). A blank sample (DI water) was chemical shrinkage was assessed following ASTM C1608 (pro-
also analyzed and used as a background correction. cedure A) (ASTM 2012c). Temperature for shrinkage study was
Once water contacts the UCP, the hydration reactions begin. controlled at 23°C (73°F) by placing vials containing the materials
Stages of the hydration process, shown in Fig. 2, occur in four into a temperature controlled water bath. The pastes were mixed at
distinct stages: (1) the dissolution stage, (2) the nucleation stage, the w/c value of 0.4. The shrinkage data were recorded every 5 min
(3) the precipitation stage, and (4) the continuing precipitation/ using an optical camera and automated data acquisition system.
dissolution stage (Odler 2008). The dissolution stage (Stage I) is
referred to as the stage when ions from the UCP dissolve in Statistical Data Analysis
solution. The ion concentrations significantly increase and reach
supersaturated conditions. The nucleation stage (Stage II) is an in- Statistical analyses of two sample t-test and analysis of variances
duction stage that allows ions to interact with each other before (ANOVA) were performed to evaluate the sample means with two
forming a new hydrated product. In this stage, the ion concentra- groups and more than two groups, respectively. The Shapiro-Wilk
tions remain at the maximum levels. Immediately after hydrated test was used to determine if the distribution of data was normal and
products begin to form, the system moves into the precipitation the Levene’s test was used to determine if the data had equal vari-
stage (Stage III). In this stage, the ion concentration decreases ance before the analyses. The statistical hypotheses are defined as
due to the consumption of ions forming new hydrated products. Null hypothesis ðH0 Þ∶μ1 ≠ μ2 ¼ · · · ¼ μa ð2Þ
The concentrations of ions then stabilize and this stage is referred
to as the continuous dissolution/precipitation stage (Stage IV).
Eventually, the rate of dissolution/precipitation of ions is reduced. Alternative hypothesis ðHa Þ∶μ1 ≠ μj for some i ≠ j ð3Þ
This is reported to be due to (1) the lack of smaller UCP, (2) the lack
of water at the cement grain surface, and (3) the lack of space The 95% confidence interval was used in the analyses in this
(Bullard et al. 2011). Faster dissolution, nucleation, and/or precipi- study. If the H0 is rejected (p-value ≤0.05), it can be concluded
tation tend to result in further reduction in flow, accelerated setting that there is a statistically significant difference at the 5% level
time, and higher chemical shrinkage values. between the means of group population. Alternatively, if the H0
The rates of dissolution (Rd ) and precipitation (Rp ) of ions in is not rejected (p-value >0.05), it can be concluded that there is
this study was determined as follows: no statistically significant difference at the 5% level between the
means of group population.

Experimental Results and Discussion


Stage II

Ion Concentration
Unhydrated PC consists of large amounts of soluble alkali com-
Stage III pounds. Once contacted with water, the pH level of the solution
rapidly increases and remains high (Rothstein et al. 2002). This
Stage IV pH affects the solubility of alkali compounds in PC systems
Stage I (Nordstrom and Munoz 2006) and can affect the hydration process.
Figs. 3(a and b) show the effects of mixing time and number of
mixer revolutions on the OH ion concentration in solution, respec-
tively. Results in Fig. 3(a) indicate that the OH ion concentration in
solution mixed at 400 rpm increases with increasing mixing time
(up to 240 min). Results in Fig. 3(b) also indicate that the OH ion
Time concentration increases as the number of mixer revolutions
increases (up to approximately 150,000 revolutions). The results
Fig. 2. Hydration process of ions in cement systems: dissolution
indicate that the OH ion concentration increases rapidly at early
(Stage I), nucleation (Stage II), precipitation (Stage III), and continuous
ages and lower number of mixer revolutions and then stabilizes
dissolution/precipitation (Stage IV)
(e.g., logarithmic function).

© ASCE 04016094-4 J. Mater. Civ. Eng.

J. Mater. Civ. Eng., 04016094


40 50

40 12.5
30 12.5

30
20
20

10 12
12 10
400 rpm
11 11
0 0
0 100 200 300 0.0E+00 5.0E+04 1.0E+05 1.5E+05
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(a) Mixing time (min) (b) Number of mixer revolutions

Fig. 3. Effect of (a) mixing time; (b) number of mixer revolutions on concentration of OH ions

20 the number of mixer revolutions does influence the Rd , but the


number of mixer revolutions higher than zero does not significantly
influence the Rd .
15 Figs. 5(a and b) show the plots of mixing time and number of
mixer revolutions versus Al ion concentration in solution, respec-
tively. Results indicate that the Al ion concentration in solution
10 mixed at 400 rpm significantly increases with increasing mixing
time from 0 to 15 min and then rapidly decreases after mixing
for 15 min to a stable level. The result of the OH ion concentration
5
as a function of number of mixer revolutions, as shown in Fig. 5(b),
exhibits a similar trend with the result in Fig. 5(a). The Al ion con-
0 centration increases, decreases, and then stabilizes with increasing
0.0E+00 5.0E+04 1.0E+05 1.5E+05 2.0E+05 number of mixer revolutions.
Number of mixer revolutions The plot of the Rd and Rp of the Al ion concentration in
solutions mixed at different numbers of mixer revolutions is shown
Fig. 4. Effect of number of mixer revolutions on Rd of OH ions
in Fig. 6. Results indicate that the Rd of Al ions increases with
increasing number of mixer revolutions. The Rd of Al ions in so-
lutions mixed at 168,000 and 336,000 revolutions are 29 and 37%
Fig. 4 shows the effect of number of mixer revolutions on the Rd higher than the Rd of Al ions in solution without mixing (mixed at 0
of OH ions in solution. Results indicate that the Rd of OH ions is revolution), respectively This indicates that there is a significant
influenced by number of mixer revolutions. The Rd for the solution difference in means. Results also indicate that the Rp of Al ions
mixed at 0; 96,000; and 192,000 revolutions are 8.4, 16.8, and in solution mixed at 168,000 revolutions is not significantly differ-
16.2 mmol=l=min, respectively. These results indicate that the ent from the Rp of Al ions in solution mixed at 336,000 revolutions.
Rd in solution mixed at 96,000 revolutions is similar to the Rd These results indicate that Rd is influenced by number of mixer
in solution mixed at 192,000 revolutions. The Rd of the OH ions revolutions but Rp is not.
in solution mixed at 96,000 and 192,000 revolutions are 100 and The effects of mixing time and number of mixer revolutions on
93% higher than the Rd of OH ions in solution without mixing the Rd and Rp of Ca ion concentration in solutions are shown in
(mixed at 0 revolution), respectively. This likely indicates that Figs. 7(a and b), respectively. Results indicate that the Ca ion

0.6 0.6

0.4 0.4

0.2 0.2

400 rpm
0 0
0 100 200 300 400 500 0.0E+00 1.0E+05 2.0E+05 3.0E+05 4.0E+05 5.0E+05
(a) Mixing time (min) (b) Number of mixer revolutions

Fig. 5. Effect of (a) mixing time; (b) number of mixer revolutions on concentration of Al ions

© ASCE 04016094-5 J. Mater. Civ. Eng.

J. Mater. Civ. Eng., 04016094


0.04 5
Rd
Rd 4
0.03

3
0.02
2
0.01
Rp 1
Rp
0
0.0E+00 1.0E+05 2.0E+05 3.0E+05 4.0E+05 5.0E+05 0
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0.0E+00 1.0E+05 2.0E+05 3.0E+05 4.0E+05 5.0E+05


Number of mixer revolutions
Number of mixer revolutions
Fig. 6. Effect of number of mixer revolutions on Rd and Rp of Al ions Fig. 8. Effect of number of mixer revolutions on Rd and Rp of Ca ions

concentration in solution mixed at 400 rpm tends to increase and particle size). Takada (2004) reported that as cement particles become
achieve maximum concentration (34 mmol=L) when the solution smaller because of abrasion during mixing process, these particles
was mixed for 180 min. After achieving the maximum concentra- can influence the hydration reaction rates.
tion, the Ca ion concentration stabilizes. In Fig. 7(b), results Results in this study indicate that the mixing time and number of
indicate that the concentration of Ca ions first increases with mixer revolutions do influence the concentrations of both Al and
increasing number of mixer revolutions and then decreases. Ca ions in solutions. Results also indicate that the Al and Ca ion
The concentration then increases again to a maximum level concentrations begin to increase at the early ages and then decrease
(36 mmol=L) at 120,000 revolutions. After increasing to the and stabilize at later ages. Furthermore, the number of mixer
maximum level, the Ca ion concentration decreases and stabilizes. revolutions does influence the Rd of Al and Ca ions, but does
The influence of number of mixer revolutions on the Rd and Rp not influence the Rp .
of Ca ion concentration in solutions is shown in Fig. 8. Results
show similar trends to the results of the Rd and Rp of Al ion con-
centration in Fig. 6. The Rd of Ca ions increases with increasing Flowability
number of mixer revolutions. The Rd of Ca ions in solution without The effect of the flowability of fresh cement mortars mixed at
mixing are 65 and 66% lower than the Rd of Ca ions in solutions 285 rpm and with different w/c values of 0.4 and 0.485 as a func-
mixed 168,000 and 336,000 revolutions, respectively. The Rp of Al tion of mixing time is shown in Fig. 9(a). Results indicate that
ion concentration in solution mixed at 168,000 revolutions shows increased mixing time results in a significant reduction in flow
no significant difference from the Rp of Al ion concentration in and the mixtures with higher w/c values exhibit higher flow values.
solution mixed at 336,000 revolutions. Frigione and Marra Dewar and Anderson (1992) reported that decreased flow likely
(1976) reported that increasing mixing speed or number of mixer occurred because of (1) inadequate water in the mixture propor-
revolutions leads to increased rate of hydration reactions and Rd of tions, (2) increased water evaporation rates, and/or (3) increased
Ca ions. In fact, results herein indicate that the Rp of Ca ions is not hydration reactions rates. Note that the testing shown in
significantly influenced by increasing number of mixer revolutions, Fig. 9(a) was discontinued at 60 min because the mortars became
but the Rd is. stiffened and uncastable. Many previous studies on concrete mixed
As discussed, the hydration reactions are controlled by both the in the field (Baskoca et al. 1998; Kirca et al. 2002; Nehdi and
dissolution stage (Stage I in Fig. 2) and the precipitation stage (Stage Al-Martini 2009) have reported that increasing mixing time
III in Fig. 2). However, the hydration reaction rates can be affected by resulted in reduced workability of fresh concrete mixtures, which
constituent material variables (e.g., paste temperature and cement is expected.

40 40

30 30

20 20

400 rpm
10 10
0 100 200 300 400 500 0.0E+00 1.0E+05 2.0E+05 3.0E+05 4.0E+05 5.0E+05
(a) Mixing time (min) (b) Number of mixer revolutions

Fig. 7. Effect of (a) mixing time; (b) number of mixer revolutions on concentration of Ca ions

© ASCE 04016094-6 J. Mater. Civ. Eng.

J. Mater. Civ. Eng., 04016094


8 200 8 200

w/c = 0.485 w/c = 0.485


w/c = 0.4 w/c = 0.4
7 7

_ 150
6 6
_
150

5 5
285 rpm

4 100 4 100
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0 20 40 60 80 0 5,000 10,000 15,000 20,000


(a) Mixing time (min) (b) Number of mixer revolutions

Fig. 9. Effect of (a) mixing time; (b) number of mixer revolutions on flow of mixtures at different w/c values

The relationship between the number of mixer revolutions The reductions of the initial setting times of the pastes with the
versus flow of fresh cement mortars with different w/c values of w/c value of 0.3 mixed at longer mixing times and higher numbers
0.4 and 0.485 is shown in Fig. 9(b). Results indicate that the flow of mixer revolutions, shown in Figs. 10(a and b), correlate with
value of fresh mortars reduces with increasing number of mixer paste temperature [Figs. 11(a and b)]. When mixing time and/or
revolutions. Results also indicate that the flow of the fresh mortars number of mixer revolutions increase, the temperature of the pastes
with lower w/c values is lower than the mortars with higher w/c with the w/c of 0.3 increases. The average temperature of the pastes
values. with the w/c value of 0.3 mixed for 2 to 60 min and from 355 to
25,435 revolutions increased by approximately 0.13°C=min
(0.23°F=min) and 3.2 × 10−4 °C=rev (5.5 × 10−4 °F=rev), respec-
Setting Time tively. Kirca et al. (2002) investigated the extended mixing of
Figs. 10(a and b) show the plots of the initial setting times for pastes concrete in the field and reported that the increase of concrete
with the w/c values of 0.3 and 0.4 mixed for different mixing times temperature from approximately 77–82°F (25–28°C) resulted
and numbers of mixer revolutions, respectively. Results shown in in a 66% reduction in workability. Baskoca et al. (1998) also in-
Fig. 10(a) indicate that the initial setting time of cement pastes with vestigated ready-mixed concrete with admixtures and reported that
a w/c value of 0.4 increases with increasing mixing time. However, the concrete temperature increased from approximately 25–29°C
the initial setting time of cement pastes with a lower w/c value (0.3) (77–84°F) mixed for 90 min and 135 revolutions. Rupnow et al.
increases with increasing mixing time from 2 to 30 min, but then (2007) reported that increased mixing time results in increased im-
decreases with increasing mixing time from 30 to 60 min. Results pact and friction, resulting in more heat generated. This leads to
in Fig. 10(b) exhibit similar trends to the results in Fig. 10(a). increased rates of hydration reactions and shorter setting times.
Results indicate that the initial setting time of cement pastes with As shown in this study, increased number of mixer revolutions also
higher w/c values tends to increase as a function of number of increased heat.
mixer revolutions. Increasing the number of mixer revolutions of As shown in Figs. 10(a and b), the initial setting times of cement
the pastes with lower w/c values from 210 to 8,330 revolutions pastes with higher w/c values (e.g., w/c value of 0.4) significantly
results in an increase of the initial setting time, but increasing increase with increasing mixing time and/or number of mixer
the number of mixer revolutions from 8,330 to 25,435 revolutions revolutions. This is likely because the temperature of pastes with
results in a reduction of the initial setting time. In addition to the the w/c value of 0.4 does not significantly increase with
initial setting times, the final setting times had a similar pattern with increasing mixing time and/or number of mixer revolutions
the initial setting times. [Figs. 11(a and b)]. The average temperature of cement pastes with

350 350

300 300

250 250

200 200

150 150

100 100
w/c = 0.4 w/c = 0.4
50 w/c = 0.3 50 w/c = 0.3
285 rpm
0 0
0 10 20 30 40 50 60 70 0 5,000 10,000 15,000 20,000
(a) Mixing time (min) (b) Number of mixer revolutions

Fig. 10. Effect of (a) mixing time; (b) number of mixer revolutions on initial setting time of mixtures at different w/c values

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85 _ 29 85 _
29
w/c = 0.4 w/c = 0.4
80 w/c = 0.3
80 w/c = 0.3

_
75 24 75 _ 24

70 70
285 rpm
_ 19 _ 19
65 65
0 10 20 30 40 50 60 70 0 5,000 10,000 15,000 20,000
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(a) Mixing time (min) (b) Number of mixer revolutions

Fig. 11. Effect of (a) mixing time; (b) number of mixer revolutions on temperature of mixtures at different w/c values

5.2 80
4.2 65
P3 - 14.5 min; 2030 rev P2 – 1.5 min; 355 rev
P4 - 14.5 min; 4060 rev
3.9 3.8

P1 – 1.5 min; 210 rev


2.6 40 3.4 52.5

1.3 3

0 0 2.6 40
0 25 50 75 100 0 1000 2000 3000 4000 5000
Hydration time (hours) Hydration time (hours)

Fig. 12. Effect of mixing time and number of revolutions on chemical Fig. 13. Effect and number of revolutions on chemical shrinkage at
shrinkage (w=c ¼ 0.4) 45 h (w=c ¼ 0.4)

the w/c value of 0.4 increases by 0.016°C=min (0.033°F=min) or (e.g., logarithmic function). Note that the chemical shrinkage of
3.9°C=rev (7.9e − 5°F=rev). Results indicate that more water likely the pastes mixed between the number of mixer revolutions lower
leads to lower friction and impact, reduced heat, and extended set- than 300 and higher than 300 is not significantly distinguished. The
ting time. In addition, this increase of heat can result in increased number of truck-drum revolutions of 300 limited by SHAs and
early compressive strength and reduced later compressive strength, specifications is not related to significant change in chemical
as reported in Prasittisopin and Trejo (2014). The heat is believed to shrinkage.
be one of the factors affecting characteristics of PC systems.
Adding additives that control the released heat can definitely extend Correlation of R d and R p of Ions with Early-Age
the set and improved later-age characteristics. Characteristics of Mixtures
This section provides correlations of the Rd and Rp of ions with the
Chemical Shrinkage
early-age characteristics of the mixtures as increasing number of
The relationship of mixing variables on chemical shrinkage at early mixer revolutions, and also discusses possible causes relating to
ages is shown in Fig. 12. The chemical shrinkage of specimens with these correlations. The Rd of OH, Al, and Ca ions has a positive
a w/c value of 0.4 and mixed for different mixing times (2 and correlation on the flowability loss and chemical shrinkage.
15 min) and numbers of mixer revolutions (210; 355; 2,030; However, there is no correlation between Rd of these ions on
and 4,060 revolutions) is shown in the figure. Results indicate that the setting time. The Rp of the ions does not correlate with the
chemical shrinkage value increases mainly with number of mixer early-age characteristics (i.e., flow, setting time, and chemical
revolutions. The increase of chemical shrinkage value is likely shrinkage). Increased Rd of ions allows the UCP to dissolve into
caused by increased hydration reaction rates. The hydration reac- solution faster, which can increase the hydration reaction rates,
tion rates increase because of an increase of paste temperature. consequently resulting in accelerated flowability reduction and
Fig. 13 shows the effect of number of mixer revolutions on chemical shrinkage. However, the Rp of Al and Ca ions does
chemical shrinkage at 45 h. Results indicate that increased number not influence the flow, setting time, and chemical shrinkage of
of mixer revolutions results in increased chemical shrinkage the mixtures. It is believed that the material variables such as
value at 45 h. The chemical shrinkage increases rapidly at lower temperature seem to have higher influence on the early-age
revolutions and then increases slowly at higher revolutions characteristics.

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J. Mater. Civ. Eng., 04016094


Conclusions ASTM. (2013). “Standard specification for standard sand.” ASTM
C778-13, West Conshohocken, PA.
Many SHAs and specifications limit the discharge time and/or ASTM. (2014). “Standard practice for mechanical mixing of hydraulic
truck drum revolutions for ready-mixed concrete. Limited research cement pastes and mortars of plastic consistency.” ASTM C305-14,
has been done to deliver whether these limits (i.e., 90-min West Conshohocken, PA.
discharge time and 300 truck drum revolutions) are applicable. Baskoca, A., Ozkul, M. H., and Artirma, S. (1998). “Effect of chemical
The results from this research indicate that: admixtures on workability and strength properties of prolonged agitated
concrete.” Cem. Concr. Res., 28(5), 737–747.
• The rate of dissolution (Rd ) of OH, Al, and Ca ions increased
Bullard, J. W., et al. (2011). “Mechanisms of cement hydration.” Cem.
with increasing number of mixer revolutions; increasing number Concr. Res., 41(12), 1208–1223.
of mixer revolutions had no influence on the rate of precipitation Charonnat, Y., and Beitzel, H. (1997). “Report: Efficiency of concrete
(Rp ) the Al and Ca ions. The Rd of ions had a positive mixers towards qualification of mixers.” Mater. Struct., 30(S1), 28–32.
correlation with the hydration reaction rates and consequently Dewar, J. D., and Anderson, R. (1992). Manual of ready mixed concrete,
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resulted in the reduction in flow and chemical shrinkage, but 2nd Ed., Blackie Academic and Professional, Glasgow, U.K.
not setting time; Diamond, S. (2005). “The patch microstructure in concrete: Effect of
• As the mixing time increased, the rate of flow reduction was not mixing time.” Cem. Concr. Res., 35(5), 1014–1016.
dependent on w/c of mixtures, but as the number of mixer Ferraris, C. F. (2001). “Concrete mixing methods and concrete mixers:
revolutions increased, the rate of flow reduction was affected State of the art.” J. Res. Natl. Stand. Technol., 106(2), 391–399.
by the w/c of mixtures. Higher w/c resulted in lower rate of flow Frigione, G., and Marra, S. (1976). “Relationship between particle size
reduction when number of mixer revolutions increases; and distribution and compressive strength in portland cement.” Cem. Concr.
• Increased number of mixer revolutions resulted in increased Res., 6(1), 113–127.
Hooton, R. D. (2008). “Bridging the gap between research and standards.”
paste temperature of the systems, likely leading to increased
Cem. Concr. Res., 38(2), 247–258.
hydration reaction rates, shorter setting times, and higher
Kirca, O., Turanli, L., and Erdogan, T. Y. (2002). “Effect of retempering
chemical shrinkage value at early ages. on consistency and compressive strength of concrete subjected to pro-
Test results for this study can provide for better understanding longed mixing.” Cem. Concr. Res., 32(3), 441–445.
of the relationships of the mixing time and number of mixer Lowke, D., and Schiessl, P. (2007). “Effect of mixing energy on fresh
revolutions on the early-age characteristics of PC systems. The properties of SCC.” Technical Univ. of Munich, Centre of Building
Rd of ions and materials temperature are correlated with hydration Materials, Munich, Germany.
reaction rates and consequently result in a change in mixture Mindess, S., Young, J. F., and Darwin, D. (2002). Concrete, 2nd Ed.,
performance at early ages. Together with the hardened character- Prentice Hall, NJ.
istics results published in Prasittisopin and Trejo (2014), their Nehdi, M., and Al-Martini, S. (2009). “Coupled effects of high tempera-
hardened characteristics also perform in the same manner as the ture, prolonged mixing time, and chemical admixtures on rheology of
early-age characteristics. fresh concrete.” ACI Mater. J., 106(3), 231–240.
Nordstrom, D. K., and Munoz, J. L. (2006). Geochemical thermodynamics,
2nd Ed., Blackburn Press, Palo Alto, CA.
Acknowledgments Odler, I. (2008). Hydration, setting and hardening of portland cement, in
Lea’s chemistry of cement and concrete, P. C. Hewlett, ed.,
This study was supported by the Washington Department of Butterworth-Heinemann, Burlinton, MA.
Transportation (WSDOT) as part of the project, Extended Prasittisopin, L., and Trejo, D. (2013). “Effects of mixing and transporta-
Discharge Time and Revolution Count for Cast-In-Place Concrete. tion on characteristics of cementitious systems containing fly ash.”
World of Coal Ash Conf., Univ. of Kentucky Center for Applied Energy
Research, Lexington, KY, 1–17.
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