Asian Journal of Civil Engineering

Influence of the variation of the content of the sand in the formation of the air bubbles
concretes with air-entraining addictive and in the its carbonation
--Manuscript Draft--

Manuscript Number: AJCE-D-19-00530

Full Title: Influence of the variation of the content of the sand in the formation of the air bubbles
concretes with air-entraining addictive and in the its carbonation

Article Type: Original Paper

Funding Information:

Abstract: Air-entraining additives are used in civil construction, for an action of elimination of the
freeze/thaw cycle, in self supporting concrete and to change its density, to obtain a
more economical structure or better thermal performance. Indented characteristics
depend on the composition of the raw materials, which in turn depend on the type,
quantity and distribution of solids and voids. Granulometric distribution of the sand,
have great influence in the formation of the air-entrained bubbles, interfering in the
quantity, size and distribution. In this study, were prepared samples using basaltic
crushed stone, Portland cement, air-entraining additive (0.5% of the cement mass) with
different levels of quartz sand, understand their influence on bubble formation. Thus, 3
types of concretes were studied: A1(1.0:1.0:2.0:0.58); A1.5(1.0:1.5:2.0:0.58);
A2.5(1.0:2.5:2.0:0.58) and A3(1.0:3.0:2.0:0.58) (cement:sand:crushed stone:w/c) and
casted in cylindrical samples of each of the respective types, cured for 7 days and
tested by water absorption, voids index and compressive tests. Amount, size,
characteristics of the bubbles entrained into the concretes, were analyzed by optical
microscopy. The connectivity of the bubbles formed was studied by exposing the
samples in a saturated chamber with CO 2 for 7, 14 and 28 days by the mensuration
of the depth of the front of carbonation. The study showed that the variation of the sand
quantity used has a great influence on the characteristics of the bubbles formed and,
there is a limit that, if exceeded, increases the possibility of its coalescence occurring
enabling it’s connection, leading to risks related to durability of the concrete.

Corresponding Author: Antonio de Paulo Peruzzi, Ph.D.

Universidade Federal de Uberlandia
Uberlândia, Minas Gerais BRAZIL

Corresponding Author Secondary

Information:

Corresponding Author's Institution: Universidade Federal de Uberlandia

Corresponding Author's Secondary

Institution:

First Author: Antonio de Paulo Peruzzi, Ph.D.

First Author Secondary Information:

Order of Authors: Antonio de Paulo Peruzzi, Ph.D.

Joseph Salen Barbar, Ph.D.

Antonio Carlos dos Santos, Doctos Professor

Daniel Soares França, graduate

Lucas Nunes Almeida, student

Order of Authors Secondary Information:

Author Comments: The results of our research show that there is an important correlation between the
number and characteristics of bubbles and their connectivity representing risks to the
durability of concrete, contrary to the theory and common sense that judges bubbles
entrained without connection.

Suggested Reviewers: Carlos Eduardo Marmorato Gomes, Ph.D.

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 Doctor Professor, Universidade Estadual de Campinas
cemgomes@fec.unicamp.br
Expert in area

Valdirene Maria Silva Capuzzo, Ph.D.

Doctor Professor, Universidade de Brasilia Centro de Desenvolvimento Sustentavel
valdirenemaria@unb.br
Expert in carbonation

João Adriano Rossignolo, Ph.D.

Doctor Professor, Universidade de Sao Paulo
j.a.rossignolo@gmail.com
Expert in light concrete

João Fernando Dias, Ph.D.

jdias@ufu.br
Expert in composite materials

Fernando Menezes Almeida Filho, Ph.D.

Doctor Professor, Universidade Federal de Sao Carlos Centro de Ciencias Exatas e de
Tecnologia
ALMEIDAFILHO@ufscar.br
Expert in concrete

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Influence of the variation of the content of the sand in the formation of the air
1
bubbles concretes with air-entraining addictive and in the its carbonation
2
Antonio P. Peruzzi (1)* ; Joseph S. Barbar (1); Antonio C. Santos (1); Daniel S. França (2); Lucas N. Almeida (3)
3
4
5
6 Abstract
7 Air-entraining additives are used in civil construction, for an action of elimination of the freeze/thaw cycle, in
8 self supporting concrete and to change its density, to obtain a more economical structure or better thermal
9
10
performance. Indented characteristics depend on the composition of the raw materials, which in turn depend
11 on the type, quantity and distribution of solids and voids. Granulometric distribution of the sand, have great
12 influence in the formation of the air-entrained bubbles, interfering in the quantity, size and distribution. In this
13 study, were prepared samples using basaltic crushed stone, Portland cement, air-entraining additive (0.5% of
14 the cement mass) with different levels of quartz sand, understand their influence on bubble formation. Thus, 3
15 types of concretes were studied: A1(1.0:1.0:2.0:0.58); A1.5(1.0:1.5:2.0:0.58); A2.5(1.0:2.5:2.0:0.58) and
16 A3(1.0:3.0:2.0:0.58) (cement:sand:crushed stone:w/c) and casted in cylindrical samples of each of the
17 respective types, cured for 7 days and tested by water absorption, voids index and compressive tests. Amount,
18
size, characteristics of the bubbles entrained into the concretes, were analyzed by optical microscopy. The
19
20 connectivity of the bubbles formed was studied by exposing the samples in a saturated chamber with CO 2 for
21 7, 14 and 28 days by the mensuration of the depth of the front of carbonation. The study showed that the
22 variation of the sand quantity used has a great influence on the characteristics of the bubbles formed and, there
23 is a limit that, if exceeded, increases the possibility of its coalescence occurring enabling it’s connection,
24 leading to risks related to durability of the concrete.
25
26 Keywords: Concrete; Air-entrained; Optical microscopy; Microbubbles; Aggregate variation
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48 (1) Professor Doctor, Faculty of Civil Engineering, Universidade Federal de Uberlandia, Av. Joao Naves de Avila, 2121
49 - Santa Monica, Uberlandia, Brazil.
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51 (2) Civil Engineering student, Universidade Federal de Uberlandia, Av. Joao Naves de Avila, 2121 - Santa Monica,
52 Uberlandia, Brazil.
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54 (3) Civil Engineering graduate, Universidade Federal de Uberlandia, Av. Joao Naves de Avila, 2121 - Santa Monica,
55 Uberlandia, Brazil.
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57 (*) e-mail autor: aperuzzi75@gmail.com
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59 ORCID ID: A. P. Peruzzi (http://orcid.org/0000-0002-0948-7930)
60 A. C. Santos (https://orcid.org/0000-0001-9019-4571)
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 Introduction
1
2
Air-entraining additives (Eair) are used in civil construction, compulsorily for an action of control of the
3 freeze/thaw cycle, but also are used in other types of situations in which the use results in technical advantage
4 like self supporting concrete, or by a lower density to obtain a more economical structure, or better thermal
5 performance. Cast-in-situ reinforced concrete is a good example of this, because has been used in many places
6 around the world as an exterior sealer and represents an economic and quick alternative to masonry or panel
7 systems due to its versatility. Thermal Conductivity (k) of ordinary concrete ranges between 1.4 and 3.6
8 W/m.K, and that represents a poor thermal performance regarding the building interior. Peruzzi, Rossignolo
9 and Kahn (2018) obtained air-entrained concretes with density 2,040kg/m3, fc = 33 MPa and k = 0.72 W/m.K,
10
that match a similar k to ceramic bricks, showing that it is possible to obtain the proper thermal performance
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12 for this building system .
13 Theoretically, the purposely air-entrained bubbles in the concretes are isolated from each other (not connected),
14 this way it does not represent risks to the durability (Neville, 2016). However, there seems to be a limit to the
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amount of air incorporated (Peruzzi, Rossignolo and Kahn, 2018) because once it is exceeded, the bubbles can
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17 rupture or fuse with each other, representing the coalescence phenomena, making the connection possible
18 (Piekarczyk, 2013) and denoting risks to the durability.
19 On the other hand, several factors interfere at the quantity and quality of bubbles formed by air-entraining
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additives (Eair), such as: the amount of Eair additive, type of mixer and mixing time, and the composition of the
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22 concrete. Therefore, this paper aimed to analyze the influence of the sand quantity variation on the
23 characteristics, quantity, distribution of the air bubbles and their connectivity. For this purpose, only the
24 proportion of fine aggregate (sand) was varied, while setting fix the type and amount of additive Eair, the mixing
25 time and using a single mixer with constant speed. The amount and characteristics of the bubbles formed were
26 studied with the aid of an optical microscope and according to the methodology proposed by Barbar (2016).
27 Connectivity of the air bubbles formed and its possible compromising effect in the concrete structure durability
28 was studied by exposing the samples in a saturated carbonation chamber of CO2 (accelerated carbonation) for
29 7, 14 and 28 days, and the depth of the front of the carbonation was evaluated. The option to use the accelerated
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process, and the saturated carbonation chamber is based on the fact that a high CO2 concentration will not
32 change the carbonation process at all, since carbonation will occur instantly, the only effect of the high CO 2
33 concentration is a faster transport of the CO2 molecules to the pore air–pore solution interface and thus a faster
34 reaction process (Visser, 2013). Thus, by studying the carbonation front it also was studied the possible
35 connectivity of the bubbles (as already mentioned), and also the durability of concrete.
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38 Experimental Procedure
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40 Materials and Methods
41 Portland cement (OPC) used for the type III (ASTM C150) has a Density (ρ) of 3.12 g/cm³ and Fc28 = 39 MPa.
42 Quartz Sand used has ρ = 2.64 g/cm³ (ABNT NM 52:2009), basaltic crushed stone (#9.5 mm or #3/8”) ρ = 2.70
43
g/cm³ (ABNT NM 53:2009). The additive Eair used was an aqueous dispersion based on resin acids and rosin
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45 acids, fumaric acids and sodium salts, with pH 10 - 12 and ρ varying between 1.010 – 1.050 g/cm3.
46 Was prepared four different types of samples of concrete with OPC, sand, crushed stone, w/c 0.58 and 0.5%
47 (cement weight) of additive Eair, whereupon the amounts of sand varied. These materials were mixed in the
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mixer for 2 minutes, resulting in the concrete samples A1, A2, A2.5 and A3 their proportions, in weight, is
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50 showed at Table 1.
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Table 1 Proportions of cement, sand, crushed Stone (in weight) and water/cement of the types of samples
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54 Type of OPC Sand Crushed Water /
55 sample Stone cement
56 A1 1.0 1.0 2.0 0.58
57 A2 1.0 2.0 2.0 0.58
58 A2.5 1.0 2.5 2.0 0.58
59 A3 1.0 3.0 2.0 0.58
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62 2
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 For each type of sample cylindrical specimens (diameter ϕ = 50mm and height h = 100mm) were prepared as
recommended by ASTM C34-13, with a demolding time of 24h, next they were kept immersed in water
1 saturated with Ca(OH)2 for 7 days, to determinate the density (ρ), water absorption ratio, and volume of voids
2 in hardened concrete (ASTM C642-13) three specimens were used for each sample type. Compressive strength
3 was determinated as recommended by ASTM C642-13, using six specimens for each sample type. “Efficiency
4 factor” (EF) has been used to classify a structural lightweight concrete by fc / ρ (MPa.dm3/kg).
5
6 For the optical microscopic analyses, were used two cylindrical specimens of ϕ = 50mm and h = 100mm (for
7 each sample type), from which they were cut at 37.5 mm from the top and at 37.5 mm from the bottom (Fig.
8 1).
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23 Fig 1 Cut surfaces by circular saw
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Specimens with cubic shape 25 x 25 x 25 (mm) were originated (Fig. 2), then the surfaces I and II were marked
27 (on the corresponding cut surface), and the surface I was used for optical microscope analyses.
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43 Fig 2 Cut surfaces by circular saw
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46 Using a metallographic sander (150 to 2500 mesh) guaranteed flatness and then the specimens were polished
47 to remove impurities, resulting in cubic specimens and ensuring the desired analysis surface as shown Fig. 3.
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61 Fig. 3 Example of cubic specimens for the optical microscope
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 Images acquired by the microscope with a magnification of 50x (Fig. 4), made it possible to observe the
1 bubbles that were delimited, using a Pro Image Express software tool to measure and quantify them for each
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specific section, according to Barbar (2016).
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19 Fig. 4 Scheme of images obtained by software Image Pro Express
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The radium of the circumferences was recorded in tables generated by the program itself and later transcribed,
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23 obtaining the respective diameters and areas used to obtain and analyze the results.
24 Accelerated carbonization process began after the wet cure time and when the samples reached a relative
25 humidity of around 35%. They were placed in a hermetically sealed chamber which, after removing the internal
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air by vacuum, was saturated with carbon dioxide (CO2), having the uniformity of gas concentration inside the
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28 chamber guaranteed by circulation through internal fans. The internal relative humidity was around 70% and
29 the exposure periods used were 7, 14 and 28 days. Then, at the end of each period, each specimen for each
30 type of sample was taken into the chamber and packed with plastic film to prevent moisture loss and possible
31 advancement on the carbonation front by contact with the external environment. All specimens, in their
32 respective exposure time, were ruptured by Tensile splitting (ASTM 496-11) and subsequently sprayed with
33 phenolphthalein solution (pH indicator) (Fig. 5) to allow the determination of the carbonated depth with the
34 aid of a caliper rule.
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55 Fig. 5 Example of cylindrical specimens after ruptured and sprayed with phenolphthalein solution
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58 Statistical analysis
59 To analyze the statistic validation of the results it was used the Chauvenet criteria.
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 Results and discussion

1
Mechanical properties of hardened concrete
2 Table 2 shows the mechanical properties of the specimens.
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5 Table 2 Density (ρ), absorption after immersion (%), volume of permeable voids (%), compressive strength (fc),
6 efficiency factor (EF)
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Type of Density (ρ) Absorption Volume Fc EF (fc/ρ)
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sample (kg/m3) after immersion of Voids (MPa) (MPa.cm3/g)
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(%) (%)
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11 A1 2,150 8.2 17.6 20.0 9.3
12 A2 2,050 9.6 19.3 19.4 9.5
13 A2.5 2,090 8.0 16.7 18.9 9.0
14 A3 2,030 7.9 16.1 16.8 8.3
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17 Fig. 6 shows the Compressive Strength Fc (MPa) and Efficiency Factor (EF) (MPa.cm3/g) obtained from
18 samples A1, A2, A2.5 and A3.
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24 EF (Mpa.cm3/g)
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26 20 Fc (MPa)
27 19.4 18.9
28 16.8
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32 9.3 9.5 9
33 8.3
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A1 A2 A2.5 A3
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41 Fig 6 Compressive Strength Fc (MPa) and Efficiency Factor EF (MPa.cm3/g) obtained from samples
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45 From the results obtained is possible verify that the fc decreases as the sand quantity increases (Tab 2 and Fig.
46 6), first because the relation cement/aggregate decreases, but also because a bigger quantity of bubbles were
47 formed, and the decrease of the Density values corroborates that fact (Tab 2 and Fig. 7). However, this tendency
48
is not verified, regarding the density mainly of the sample A2.5 that has a ρ larger than A2. Figure 7 shows
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50 Density (kg/m3), and Fig. 8 shows the Absorption after immersion and Volume of Voids (%) obtained from
51 samples A1, A2, A2.5 and A3.
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 2,150
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4 2,090
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7 2,050
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9 2,030
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A1 A2 A2.5 A3
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3
18 Fig. 7 Density (ρ) (kg/m ) obtained from samples
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25 Absorption
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27 Volume of Voids
28 19.3
29 17.6 16.7
30 16.1
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33 9.6
8.2 8 7.9
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A1 A2 A2.5 A3
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42 Fig. 8 Absorption after immersion and Volume of Voids (%) obtained from samples
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45 Through the analysis of Figure 8 is possible to note that A2.5 and A3 both have close values of Absorption
46 (8% and 7.9%), but A3 has smaller Density (Fig. 7), and Fc smaller accordingly (Fig. 6), indicating that there
47 are differences in the structure of the bubbles formed, therefore the microstructural analyses can help to
48 understand this process.
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52 Microstructure analysis by Optical Microscope
53 Table 3 shows the number of bubbles formed, distributed by ranges of Diameter and the total number of
54 bubbles, analyzing the table is possible to note that the number of bubbles increases as the quantity of sand
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increases, such as expected according to the bibliography.
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 Table 3 Number of Bubbles (and percentage) obtained from the software Pro Image Express (face I of the prism)
distributed by ranges of Diameter and the Total of bubbles
1 Type of Range of diameter of Bubbles (μm) Total
2 sample 0- 100 - 200 - 300 - 400 -
>500
3 100 200 300 400 500
4 A1 518 38 5 1 0 2 564
5 (91.8%) (6.7%) (0.9%) (0.2%) (0%) (0,4%)
6 A2 80 41 12 2 2 6 143
(55.9%) (28.7%) (8.4%) (1.4%) (1.4%) (4.2%)
7
A2.5 907 83 18 7 1 7 1,023
8 (88.7%) (8.1%) (1.8%) (0.7%) (0.1%) (0.7%)
9 A3 1,056 72 19 3 1 14
10 1,165
(90.6%) (6.2%) (1.6%) (0.3%) (0.1%) (1.2%)
11
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13 In this paper we detach the range of diameters of the bubbles between two types: 1) “microbubbles” which the
14 diameter is <500 μm and the bubbles are considered small, spherical and unconnected, and 2) “macrobubbles”
15 which the diameter is >500 μm and they are formed by the mixer or transport of concrete, or product of bubble
16 coalescence. As already said, all of the samples have been made following the same procedures, varying only
17 the sand quantity, so the quantity of “macrobubbles” originated in the mixer phase are, theoretically, the same
18
in all samples, or in other words, the difference of the “macrobubbles” quantity should be product of bubble
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20 coalescence. Tab 3 shows that while the quantity of sand increases the “macrobubbles” quantity increases,
21 except in sample A2, that has been showing a different behavior when it comes to Density, Absorption, and
22 number of bubbles. Possibly as a result of the mixing phase. Table 4 shows the Area of the bubbles and the %
23 distributed by ranges of Diameter.
24
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26 Table 4 Area of the Bobbles (μm2) x 105 (and percentage) obtained from software Pro Image Express (face I of the
27 prism) distributed by ranges of Diameter
28 Type of Range of diameter of Bubbles (μm)
29 sample 0- 100 – 200 - 300 - 400 - Area Total
30 >500
31 100 200 300 400 500 (μm2) x105
32 A1 3.7 2.6 1.1 0.6 0.0 2.6 10.6
(35.0%) (24.5%) (10.4%) (5.7%) (0.0%) (24.5%)
33
34 A2 1.1 3.1 2.6 1.0 1.4 11.2 20.4
(5.4%) (15.2%) (12.7%) (4.9%) (6.9%) (54.9%)
35
36 A2.5 6.3 6.7 3.5 3.3 0.7 14.3 34.7
(18.2%) (19.3%) (10.1%) (9.5%) (2.0%) (42.2%)
37
38 A3 7.0 4.6 4.5 1.3 0.7 13,2 31,3
39 (22.4%) (14.7%) (14.4%) (4.2%) (2.2%) (42.2%)
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42
From Table 4 we can see that the area of “macrobubbles” increases as the amount of sand increases, and the
43 area at A2.5 and A3 have close values, highlighting the coalescence of the bubbles. Whether this means they
44 are connected or not, and if they can cause durability impairment, can be studied in the Carbonation front
45 analyses.
46
47 Carbonation front analyses
48
49 Table 5 shows the Carbonation front depth of the samples after 7, 14 and 28 days of Accelerated carbonization placed in
50 a hermetically sealed chamber saturated with carbon dioxide (CO2). Fig. 9 introduce these results through a bar chart.
51
52
53 Table 5 Carbonation Front Depth (mm) of the samples at 7, 14 and 28 days
54 Carbonation Front Depth
55 Type of (mm)
56 sample Days Under CO2
57 7d 14d 28d
58 A1 1.2 2.5 3.3
59 A2 3.3 4.3 5.7
60 A2.5 3.2 5.8 6.5
61 A3 4.9 6.8 7.0
62 7
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 1
2
3 7 days 14 days 28 days
4
5
6.5 6.8 7.0
6
7 5.7 5.8
8 4.9
9 4.3
10
11 3.3 3.3 3.2
12 2.5
13
14 1.2
15
16
17
18 A1 A2 A2.5 A3
19 Fig. 9 Carbonation Front Depth (mm) of the samples at 7, 14 and 28 days under Accelerated carbonation process
20
21
22 Tab 5 and Fig. 9 shows that the carbonation front depth increases as the quantity of sand is increased, and denote that
23 there is a connection between the bubbles and sand, and that it may represent risks to the durability of the concrete.
24
25
26
27 Conclusions
28
29
Incorporating sand to the air-entrained concrete significantly increases the quantity of bubbles entrained as the
30 bibliography reports, but it also improves the quality of the bubbles since it is considered that a larger amount
31 of bubbles with smaller diameter is a better condition than one with large bubbles.
32 The coalescence of the bubbles could be evidenced by the results obtained in this research, mainly related to
33
34
the number of bubbles and area of the largest bubbles, and their connection by the depth of the Carbonation
35 front.
36 Results obtained here report that there is a limit to the quantity of bubbles entrained in the concrete and,
37
if exceeded represents risks to the durability of the concrete.
38
39
40
41 Acknowledgement
42
43 The authors thank the Faculty of Civil Engineering of the University Federal of Uberlandia, specially Leticia Silveira
44 Valeriano, Cristiane Pires and Wanderly Geraldo da Silva.
45
46
47 Compliance with ethical standards
48
49 Conflict of interest On behalf of all authors, the corresponding author states that there is no conflict of interest.
50
51
References
52
53 Peruzzi, A. P.; Rossignolo, J. A., Kann,H. (2018) Air-entrained concrete: relationship between thermal
54 conductivity and pore distribution analyzed of by X-ray tomography. Journal of Civil Engineering and
55 Architecture, http://doi.org/10.17265/1934-7359/2018.07.005
56
57 Neville, A. M. (2016) Propriedades do concreto. Porto Alegre, RS: Bookman.
58
59 Piekarczyk, B. L. (2013) The type of air-entraining and viscosity modifying admixtures and porosity and frost
60 durability of high performance self-compacting concrete. Construction and building materials,
61 http://dx.doi.org/10.1016/j.conbuildmat.2012.11.032
62 8
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 Barbar, J. S. (2016) Influência do teor de ar incorporado no desempenho de concretos com diferentes teores
de agregados. Doctoral thesis. IAU-SC USP. https://teses.usp.br/teses/disponiveis/102/102131/tde-
1 23012017-100027/pt-br.php
2
3 Visser, J.H.M. Influence of the carbon dioxide concentration on the resistance to carbonation of concrete.
4 Construction and Building Materials. https://doi.org/10.1016/j.conbuildmat.2013.11.005
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