ACI JOURNAL
Title no. 80-33
Air Entrainment in the Presence of Superplasticizers
by G.G. Litvan
Air-entrained and plain mortar specimens (cement-sand ratio = 1:3,
water-cement ratio = 0.65) were prepared using a modified sulfon-
ated polymer, a naphthalene-formaldehyde condensate, or a sulfon-
ated melamine formaldehyde admixture at two levels of concentra-
tion. The air-void system determined by the linear traverse method,
the pore size distribution obtained by mercury intrusion porosimetry,
and frost resistance assessed by alternate freezing and thawing were
compared with those of control mixes containing no superplasticizer.
A large pore volume (- 0.3 to 2 I'm) in the presence of an air-en-
training admixture is assumed to be responsible for the improved
frost resistance of cement paste. Superplasticizers eliminate large air
voids visible under the microscope but do not significantly interfere
with the action of air-entraining admixtures in the formation of small
pores.
Keywords: air-entraining agents; air entrainment; freeze-thaw durability; mor-
tars (material; plasticizers; porosity; voids; water-reducing agents.
The freeze-thaw resistance of concrete containing a
superplasticizer (high-range water-reducing admixture)
has been a controversial topic for some time. t-tz Con-
cern is based on the fact that in air-entrained, super-
plasticized concrete the conventional air-entraining ad-
mixtures fail to achieve air content of six percent with
a void spacing of 0.2 mm which are considered essen-
tial for good freeze-thaw resistance. The performance
of concrete containing superplasticizer and air-entrain-
ing admixtures has been found, however, to be supe-
rior to that expected on the basis of air content and
spacing factor values. This is most surprising because
air content and, particularly, void spacing are known to
be excellent indicators of freeze-thaw resistance, and a
unique relationship is believed to exist between frost
resistance and the two parameters.
Apart from the theoretical interest, these observa-
tions are of great practical importance. Firstly, air-en-
trained concrete containing a superplasticizer admix-
ture cannot be used with complete confidence in a
freezing environment until the cause of the anomalous
behavior is identified. Secondly, prediction of perfor-
mance of plain concrete in a freezing environment is
made more uncertain by the discovery that under cer-
tain conditions the relationship between the void spac-
ing factor and frost resistance is ambiguous. The pres-
326
TECHNICAL PAPER
ent study was undertaken to gain a better understand-
ing of the effect of air-entraining admixtures in the
presence or absence of high-range water reducers.
TEST SPECIMENS
Mortar used in the fabrication of the specimens was
made of CSA Type 10, ASTM Type I portland cement,
and ungraded sand. The high-range water-reducing ad-
mixtures were as follows: a) a modified sulfonated
polymer, manufactured in Montreal, Canada; b) a
naphthalene-formaldehyde condensate manufactured in
the U.S.; and c) a sulfonated melamine formaldehyde
of German origin. The air-entraining admixture was the
triethanolamine salt of a sulfonated hydrocarbon.
The mixes were prepared in a laboratory type mixing
machine (Hobart, Model N-50) in batches containing
200 g cement in accordance with ASTM C 192 standard
method. The water-cement ratio was 0.65 and the ce-
ment-sand ratio (by weight) 1:3. The air-entraining
agent was added with the water, while the superplasti-
cizer was mixed in two minutes before the termination
of stirring. Table 1 lists the mixes together with admix-
ture concentrations, the lower values being the dosages
recommended by the manufacturers.
Prisms 25 by 25 by 150 mm, outfitted with stainless
steel studs for length change measurements, were pre-
pared by casting. Upon removal from the molds (after
1 day), the specimens were cured in a fog room for 28
days.
EXPERIMENTAL METHODS
The air void content and spacing factor was deter-
mined according to the ASTM standard recommended
practice, C 457-71Y An instrument capable of produc-
ing 41.34 MPa (60,000 psi) was used for pore size dis-
tribution analysis by the mercury intrusion method.
Received Aug. 29. 1982, and reviewed under Institute publication policies.
Copyright © 1983, American Concrete Institute. All rights reserved, including
the making of copies unless permission is obtained from the copyright propri-
etors. Pertinent discussion will be published in the May-June 1984 ACI JOUR-
NAL if received by Feb. I, 1984.
ACI JOURNAL I July-August 1983
ACI member G. G. Litvan is senior research officer of the Division of Build-
Table 1 - Admixture concentration, air content,
ing Research, National Research Council Canada. Dr. Litvan 's research deals spacing factor, and total porosity of specimens
with surface chemical problems of concrete durability. He is a corresponding I 2 3 4 5 6 7
member of ACI Commillee 201. Durability of Concrete, and technical com-
millees of CSA and RILEM. He is past president of the Eastern Ontario and Admixture Linear traverse
Quebec ACJ Chapter. Air Spacing
Cone, content, factor, Porosity,
Code Type percent' AE* percent mm percent

Resistance to rapid freezing and thawing was assessed 461 - - - 3.91 0.79 16.0
465 - - + 11.45 0.28 20.9
on duplicate specimens according to ASTM standard 462 A 0.75 - 3.99 0.69 12.3
test method C 666, 14 Procedure B, involving freezing in 466 A 0.75 + I 12.40 0.28 21.8
air and thawing in water. 463 A 1.25 - 5.09 0.76 N/A
467 A 1.25 + 13.10 0.20 21.2
464 A 2.00 - 5.32 0.71 13.2
RESULTS 459 A 2.00 + 11.10 0.20 20.5
Air contents and spacing factor determined by a mi- 469 B 0.75 - 3.59 0.74 15.2
471 B 0.75 + 8.76 0.33 19.3
croscopical method are shown in Table 1, Columns 5 470 B 1.25 - 2.48 0.94 15.7
and 6, respectively. The apparently high air content 472 B 1.25 + 8.41 0.43 19.1
values result from the absence of coarse aggregate in 473 c 1.50 - 3.01 0.86 14.0
468 c 1.50 + 8.31 0.41 19.3
the samples. It has to be remembered that in concrete 474 c 2.50 - 1.61 0.99 15.6
the air content is expressed as percentage of total vol- 475 c 2.50 + 11.13 0.28 18.6
ume, or six times larger than that of the cement paste • Air-entraining admixture.
'Weight of liquid admixture expressed as percent of cement.
(the cement-sand-aggregate weight ratio being
1:2.25:2. 75). In mortar with a cement-sand ratio of 1:3 8. Total porosity (Column 7) of air-entrained mortar
the reference volume is only four times larger than the appears to be little affected by Superplasticizer A (466,
volume of the cement paste. The following observa- 467, 459 versus 465).
tions can be made: 9. Total porosity (Column 7) of air-entrained mortar
I. Superplasticizer A increases the air content (Col- is somewhat reduced by either Admixture B or C (471,
umn 5) of non-air-entrained plain mortar (461) and this 472, 468, and 475 versus 465). Pore size distribution
effect is proportional to the concentration of Admix- curves of the specimens are shown in Fig. 1.
ture A. Superplasticizers B and C decrease the air con- 10. In general, due to air entrainment there is signif-
tent, C more than B, and this effect is concentration- icant difference in pore size distribution, mainly in the
. dependent (469, 470 and 473, 474, Column 5). region of 1 to 0.1 p.m pore diameter, regardless of the
2. The air-entraining action of Superplasticizer A is type of superplasticizer (465 versus 461; 466, 467, 459
apparent also in air-entrained specimens. Here the air versus 464, 462; 471, 472 versus 470, 469; 468, 475 ver-
content is even higher than in the plain air-entrained sus 474, 473).
specimens (466, 467, and 459) at constant dose of the 11. In air-entrained mortars, the volume of pores
air-entraining agent, and in Specimen 467 it is the high- with 1 to 0.1 p.m diameter appears in the presence of
est in the set (13.10 percent). Admixture A (466, 467, 459) to be similar to the vol-
3. In specimens containing either B or C plus an air- ume of pores in the air-entrained mortar without su-
entraining admixture the air content is considerably perplasticizer (465); in the presence of Admixtures B
greater than in the companion non-air-entrained mor- and C (471, 472, 468, 475) the pore volume appears to
tars (471, 472, 468, 475 versus 469, 470, 473, 474, re- be smaller.
spectively), but it is less than that of Specimen 465, Table 2 shows the volume of pores of selected sizes
which contains air-entraining agent but no superplasti- expressed as percentage of apparent volume. The effect
cizer. of the air-entraining admixture is measured by the in-
4. Spacing factor (Column 6) of non-air-entrained crease of the pore volume in terms of the volume of the
mortar containing Admixture A (462, 463, 464) does non-air-entrained mortar of the same class.
not show the significant difference, with respect to ref- 12. Of the four pore size ranges, <0.088, >0.088, 2
erence specimen 461, comparable to the increase in air - 0.035, and 2 - 0.35 p.m, the volume of pores be-
content (Column 5). longing to the last group increases most as a result of
5. In the presence of Superplasticizer A the addition air entrainment, whether superplasticizer is present or
of the air-entraining agent achieves or approaches the not.
required spacing factor of less than 0.2 mm (466, 467, Fig. 2(a and b), which shows the dimensional
459). changes of the specimens effected by alternate freezing
6. Air-entrainment in the presence of admixture, and thawing, leads to observations 13 to 15. Because
either B or C, produces spacing factor values (Column the curves obtained from duplicate specimens are simi-
6) that are greater than the required 0.2 mm (471, 472, lar there is only one curve for each set. Table 3 gives
468, and 475). the number of cycles producing 0.1 and 0.2 percent ex-
7. In non-air-entrained mixes total porosity is less in pansion.
the presence than the absence of superplasticizers (461 13. All air-entrained specimens, with and without
versus 462, 464, 469, 470, 473, and 474). superplasticizer, show good freeze-thaw resistance as
ACI JOURNAL I July-August 1983 327
 24 be detrimental in this respect (473, 474). These IndiCa-
tions must be treated with caution until further experi-
20 mental evidence can be obtained.
16
DISCUSSION
12 The results give clear indication that even if the spac-
ing factor is larger than 0.2 mm, good frost resistance
8
is provided by an air-entraining admixture in the pres-
4 ence of superplasticizer. This is in agreement with the
findings of previous workers. Behavior deviating from
0 that expected on the basis of the spacing factor was ob-
12 served earlier. Mielenz 15 found no general correlation
between spacing and durability factors. Rather, each
10 combination of admixtures seems to produce its own
8 relation between the two parameters.
The significant, and unique, increase of pore volume
6 in the range of 0.35 to 2 t-tm diameter found in this
study strongly suggests that pores of this size may be
""' 4
'-'-'-
responsible for the increased frost resistance of air-en-
:2' 2 trained cement paste. This hypothesis is contradictory
::::>
_, to the present view of the mechanism of protection by
0
> 0 air entrainment. The success of air entrainment, how-
>- 12 ever, has never been proved to rest on the incorpora-
1-

V'l
tion of air voids. Two facts are indisputable: Addition
10
0
0::
of air-entraining agents is beneficial, and in entrained
0
Cl.. 8 paste large voids are detectable.
Although Walker and Hsieh 16 found that the volume
6 of pores in the + 8 micron range correlate best with
freeze-thaw durability of various aggregates, Koh and
4
Kamada 17 reported a good relation between frost resis-
2 tance and the volume of pores in the 0.15 to 1.5 ttm
range, increasing greatly with the addition of air-en-
0 training agent to the mix. Lange and Modry 18 investi-
12 gated the frost resistance of limestone aggregates and
observed good performance if pore size distribution in-
10
dicated a large number of pores in the 2 to 0.2 t-tm
8 range. This is corroborated by the present work. Re-
sults obtained by Cebeci 19 also indicate that the pore
6 size distribution of air-entrained cement paste differs
4 from that of the corresponding air-free paste, mainly in
the region of 2 to 0.1 ttm pore diameter.
2 Furthermore, in an attempt to provide freeze-thaw
durability for cement paste by incorporating particu-
late matter containing pores it was found 20 that large
pores in the over 2 t-tm range of agglomerated and sin-
PORE DIAMETER, !Lm tered fly ash were, surprisingly, not effective at all. The
presence of smaller pores between 0.3 and 2 t-tm in fired
Fig. 1 - Pore size distribution of specimens deter- clay and diatomaceous earth imparted excellent frost
mined by mercury intrusion porosimetry resistance.
Kaneuji, Winslow, and Dolch 21 established a correla-
evidenced by the low values of expansion. tion between the freeze-thaw durability of coarse ag-
14. Admixture A, without air entrainment, provides gregates and their pore structure. Frost susceptibility
limited degree of frost resistance (462, 463, 464 com- was found to be associated with large total pore vol-
pared with 461) that increases with increasing admix- ume and small median diameter in the range extending
ture concentration. from 1 ttm to larger sizes.
15. Admixtures B and C provide no protection with- The role of the 0.35 to 2 t-tm diameter pores has es-
out air entrainment (469, 470, 473, 474). The number caped attention up to now because in plain concrete the
of cycles to produce 0.1 to 0.2 percent expansion is large-air-void: small-pore ratio is probably constant;
larger in the plain mix (461) than in the presence of measuring one provides information about the other. In
Admixture B. Increased concentration of C appears to the presence of superplasticizer, however, not only is
328 ACI JOURNAL I July-August 1983
the entrapped air partially eliminated, but the ratio of 3.5
air voids to small pores is also upset. 4.28 X 1012
o.817 x 10- 12
The presence of air voids larger than 10 ttm is known
to enhance frost resistance of concrete. The importance The volume of protection per sphere is
of the smaller pores of 0.3 to 2 t-tm size is due to the
much smaller spacing factor that is created for a given 100
air content. It can be shown by a simple calculation: 23.4 X 10- 12 ml
4.28 x w- 12
Assuming that 3.5 percent of the apparent volume is
in pores of 0.35 to 2 ttm diameter, then the average di-
Assuming the volume to be in the shape of a cube, the
ameter is
edge is
2 - 0.35
+ 0.35 = 1.17 ttm 423-:-4><10- 12 = 2.86 x 10- 4 em
2
The spacing between the edges of two spherical voids
The volume of a spherical shaped pore with radius r is is 2.86 - 1.17 = 1.69 t.tm, and the maximum distance
of any point in the cement paste from the periphery of
4.189 X (0.58 X 10- 4) 3 a void is 0.85 t.tm, or 120 times less than the recom-
mended distance.
0.817 X 10- 12 ml The importance of the 0.3 to 2 ttm pores, if substan-
tiated, brings into question the basis of the linear trav-
The number of spheres in paste of 100 ml apparent erse method and suggests mercury intrusion porosime-
volume is try as a more meaningful test. The latter promises to be

Table 2 - Effect of air entrainment on volume of pores of selected sizes

expressed as percentage of apparent volume
Pore
diameter .;;0.088/lm >0.088/lm 2 - 0.035/lm 2- 0.35 I'm

Volume,
Increase
as percent Volume,
Increase
as percent Volume,
Increase
as percent Volume,
I asIncrease
percent
Code percent NAE* percent NAE percent NAE percent I NAE

461 9.8 6.2 10.7 2.4

465 10.4 I 106 10.5 170 15.0 140 I 5.9 246
462 9.4 5.1 7.1 I 2.0 I
466 9.9 I 105 11.5 227 14.8 207 6.3 315
463
467 10.9 10.1 15.1 5.5
464 9.8 I 5.1 8.0 2.0
459 9.6 97 10.9 214 13.8 172 5.4 270
469 10.3 5.4 9.7 1.8
471 12.4 120 7.8 I 145 13.7 141 3.5 I 194
470 10.0 5.9 8.3 1.7
472 13.0 130 7.2 122 13.0 157 3.5 I 205
473 10.6 4.7 8.8 1.5
468 13.0 123 7.3 154 14.3 162 3.3 220
474 10.3 5.5 7.3 1.3
475 13.0 126 7.0 127 12.8 175 2.8 215
Average 115 165 164 237
• NAE = non·air·entrained.

Table 3 - Summary of results of freezing and thawing test

No. of cycles
producing Sample I Sample II Average
0.1 0.2 Expansion/ Expansion/
Percent Ultimate 100 cycles Ultimate 100 cycles Expansion/
Specimen residual expansion, Ultimate X 100, expansion, Ultimate X 100, 100 cycles
code expansion percent cycle average percent cycle average X 100

461 41 67 1.000 216 46.30 0.962 284 33.80 40.05

465 >760 >760 0.030 760 0.39 0.022 760 0.28 0.33
462 86 200 0.742 520 15.46 0.584 418 13.96 14.12
466 >760 >760 0.040 760 0.52 0.042 760 0.56 0.54
463 145 245 0.878 520 16.88 0.784 418 18.76 17.82
467 >760 >760 0.036 760 0.48 0.046 760 0.60 0.54
464 195 330 1.072 760 14.18 0.944 760 12.42 12.30
459 >760 >760 0.032 760 0.42 0.024 760 0.32 0.36
469 15 22 0.960 120 80.00 1.102 120 91.80 86.00
471 >760 >760 0.038 760 0.50 0.036 760 0.48 0.48
470 13 21 1.106 90 122.80 1.164 90 129.20 126.00
472 >760 >760 0.036 760 0.48 0.036 760 0.48 0.48
473 49 78 1.016 200 50.80 0.996 148 67.20 59.00
468 >760 >760 0.024 760 0.32 0.026 760 0.34 0.34
474 17 28 1.178 90 130.80 0.996 106 94.00 112.40
475 >760 >760 0.030 760 0.38 0.026 760 0.34 0.36

ACI JOURNAL I July-August 1983 329

 Fig. 2 - Residual expansion mortar prisms as a func-
(a) tion of alternate freezing and thawing. a) Non-air-en-
trained mixes: 461 reference, 462-464 Admixture A;

r
z
0
EXPANSION
469-470 Admixture B; and 473-474 Admixture C. b)
Air-entrained mixes: 465 reference, 466-467, 459, Ad-
mixture A; 471-472 Admixture B; and 468 and 475 Ad-
mixture C
for microscopical observation, and the procedure itself
is time consuming, demanding, and subject to operator
(/') judgement. It cannot be easily automated using an im-
z age analyzer. In contrast, mercury porosimetry can be
<(
a.. performed easily and quickly in the laboratory and is
X reproducible. It is possible that a relatively simple test
LL.J
could be developed for field test. Obviously, appropri-
ate sampling procedure will have to be devised to as-
sure representativeness in concrete.
Klieger found 22 that the strength reduction due to air
entrainment depends on cement content, aggregate size,
and amount of air-entraining agent. The representative
value at 6 percent air, 290 kg/m 3 cement content, 50 to
7 5 mm slump and 19 mm aggregate size results in a loss
of 2. 7 percent in flexural strength and, for compressive
strength, 3.9 percent per each percent of air. This sub-
stantial loss in mechanical strength is unnecessary and
can be avoided without loss of durability. Good frost
resistance appears to be possible by increasing the vol-
ume of small pores, thus avoiding the reduction of me-
chanical strength.

CONCLUSIONS
The present studies lead to the following conclu-
0 100 200 300 sions:
NUMBER OF CYCLES 1. The improved freeze-thaw resistance of air-en-
trained mortar is due mainly to the increased number of
pores with diameters in the range of 0.3 to 2 p.m.
I I I 2. Superplasticizers eliminate large air voids, but the
(b) pore volume of the critical size is still greatly and suf-
r- 465 -

r
ficiently increased by air-entraining admixtures. This
I 0.1% FRACTIONAL
-
conclusion is put forward as an explanation for the
I-
EXPANSION 466 good frost resistance of superplasticized concrete de-
spite its high spacing factor.
z I-
467 - 3. For the assessment of freeze-thaw resistance a test
0 based on measurement of the air-void content in the 0.3
(/') I- 459 - to 2 p.m diameter range could be developed; not only
z would it be more reliable but it would be simpler to
<(
a..
r- 471 - perform than the present ASTM C 457 test.
X
LL.J I- 472 - ACKNOWLEDGMENT
The competent technical help of H. Schultz in carrying out the ex-
- 468 - perimental work is gratefully acknowledged. This paper is a contri-
bution from the Division of Building Research, National Research
I- 475 - Council Canada, and is published with the approval of the Director
of the Division.
I I I
REFERENCES
0 100 200 300 I. Tynes, William 0., "Investigation of Proprietary Admixtures,
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330 ACI JOURNAL I July-August 1983

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ACI JOURNAL I July-August 1983
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331