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Cement, Concrete, and Aggregates, June 2003, Vol. 25, No.

1
Paper ID CCA11842_251
Available online at: www.astm.org

J. E. Gillott1 and T. Quinn2

Strength and Sulfate Resistance of Concrete


Made With High Alumina Cement, Type 10
Portland Cement, Type 10 Portland Cement Plus
Fly Ash and Type 50 Portland Cement

ABSTRACT: Concrete prisms and cylinders were made using four different cementitious materials. These were high alumina cement (HAC), Type
10 Portland, Type 10 with 20% replaced with fly ash and Type 50 Portland Cement. Specimens were used for measurement of length change and
estimation of compressive strength over a period of about 18 months exposure to fog-room conditions, room temperature Na2SO4 solution or 40°C
water bath. None of the concrete samples made with the 3–types of Portland–based cementitious material showed distress due to sulfate attack. The
concrete made with HAC and which had probably not undergone the conversion reaction also showed good resistance to sulfate attack but samples
in which conversion had probably occurred cracked and disintegrated in the Na2SO4 solution.

KEYWORDS: concrete, Portland binders, high alumina cement, sulfates, strength, durability

Introduction ume proportion of sulfate solution to mortar bars of 4  0.5


volumes of solution to 1 volume of mortar bars. In the present work
Concrete prisms (76  76  280 mm) and concrete cylinders
the volume proportion was about 3.3 volumes of solution to 1 vol-
(100  200 mm) were cast using four different cementitious mate-
ume of concrete prisms and the ratio was about 2.1 for solution to
rials during spring and summer of the year 2000 for a comparative
concrete cylinders. The prisms and cylinders were stored in con-
study of sulfate resistance and strength development. The main
tainers (Fig.1a) but in both cases the volume proportion was less
purpose was to use the samples and data in the 3rd and 4th year ma-
than that required by ASTM. This followed because the concrete
terials courses in civil engineering. The cementitious material in
specimens occupy a larger volume than a corresponding number of
the four different batches of concrete consisted of high alumina ce-
mortar bars and too few containers were available to compensate
ment (HAC), (calcium aluminate cement, ciment fondu), Type 10
for the difference. A review of ASTM C1012 in assessing sulfate
Portland cement,3 Type 10 Portland cement of which 20% was re-
resistance of different mortars with a view to establishing accep-
placed by Sundance fly ash (Type C)4 and Type 50 Portland ce-
tance limits was given by Patzias (1987, 1991).
ment.3 Available chemical and physical analyses and mix designs
are shown in Table 1a,b,c. The prisms were made for measurement
of length change, which was recorded in triplicate on prisms as a Objectives
function of time of immersion in room temperature Na2SO4 solu- The principal objectives of the work were as follows:
tion. The cylinders were used for estimation of compressive
strength as a function of time in the fog-room, 40°C water bath or
Na2SO4 solution. Treatment is summarized in Table 2. 1. To demonstrate to 3rd and 4th year students of civil engineer-
In ASTM C1012-95 a procedure is described that “provides a ing the effects of sulfate attack on concrete made with four
means of assessing the sulfate resistance of concretes and mortars,” types of cementitious material.
by measurement of length change of mortar bars immersed in a sul- 2. To provide students with evidence of sulfate attack in the
fate solution. The procedure used in this work differed in that con- form of:
crete, rather than mortar, test specimens were used. Also ASTM (a) Cracking and disintegration of test specimens;
C1012 calls for the use of a container large enough to allow a vol- (b) Length change of test specimens;
(c) Changes in compressive strength of test specimens.
3. To demonstrate to students:
(a) The differences in sulfate-resistance of the four types of
1
Emeritus Professor, Department of Civil Engineering, The University of concrete;
Calgary, AB T2N 1N4, Canada. (b) That evidence of sulfate resistance could be obtained
2
Technologist, Department of Civil Engineering, The University of Calgary, within a reasonably short time-frame (say 6 months) by
AB T2N 1N4, Canada. means of a “practical” easy-to-use-test.
3
CSA Standards, CAN/CSA–A5
4
CSA Standards, CAN/CSA–A23.5 4. To provide answers to several questions such as:
Manuscript received 12/13/2002; accepted for publication 4/16/2003; (a) Would modification of the standard test (ASTM C1012)
published XX. impair its utility? In this work specimens were made of

Copyright © 2003 by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. 21
22 CEMENT, CONCRETE, AND AGGREGATES

TABLE 1a—Proportions by weight (kg/m3) of ingredients in four concrete mixtures.

Ingredients

CEMENT HAC P.C. Type 10 P.C. Type 50 Fly Ash Water Coarse Agg. Fine Agg. W/cm

High Alumina 400 160 1127 620 0.4


Portland Type 10 370 185 1050 750 0.5
Type 10 Fly Ash 296 74 185 1050 750 0.5
Portland Type 50 370 185 1050 750 0.5

Abbreviations: HAC  High Alumina Cement ; Agg.  Aggregate; P.C.  Portland Cement; W/cm  Water/Cementitious Material

TABLE 2—Treatment of concrete prisms and cylinders made with high


TABLE 1b—Chemical analyses of portland cements. alumina cement and portland cementitious materials.

Cement Type Prisms: Length Change Data

Type 10 Type 50 (a) High Alumina Cement


Chemical Analysis % % Fog Room (70 Days) → Na2SO4 solution
Fog Room (3 Days) → Water bath 40°C (70 Days) → Na2SO4 solution
Silica (SiO2) 20.5 21.4 (b) Portland Cementitious Materials
Alumina (Al2O3) 4.1 3.3 Type 10
Iron Oxide (Fe2O3) 2.7 3.8 Type 10  Fly Ash → Fog Room (7 Days) → Na2SO4 solution
Calcium Oxide (CaO) 63.2 62.5 Type 50
Magnesium Oxide (MgO) 4.5 4.5
Sulphur Trioxide (SO3) 2.4 2.2 Cylinders: Compressive Strength Data
Loss on Ignition at 1050°C 2.8 ...
Loss on Ignition at 550°C 0.9 ... (c) High Alumina Cement
Loss on Ignition ... 1.0 Fog Room (18 Months)
Insoluble Residue 0.14 0.10 Fog Room (70 Days) → Na2SO4 solution
Calcium Oxide, Free (FCaO) 1.01 0.42 Fog Room (3 Days) → Water bath 40°C (18 Months)
Equivalent Alkali (As Na2O) 0.55 0.56 Fog Room (3 Days) → Water bath 40°C (70 Days) → Na2SO4 solution
C3 S 62.8 58.0 (d) Portland Cementitious Materials
C2S 11.5 17.7 Type 10 Fog Room (18 Months)
C3A 6.3 2.3 Type 10  Fly Ash → →
C4AF 8.3 11.4 Type 50 Fog Room (7 Days) → Na2SO4

TABLE 1c—Physical analyses of portland cements. of knowledge in this area since student class notes, where
these topics are covered, were not available to people in civil
Cement Type
engineering practice some of whom expressed interest in the
Type 10 Type 50
results.
Physical Analysis % %
Methodology
Fineness 45m% Retained 3.1 1.8
Blaine m2/kg 379 380 The concrete prisms made with high alumina cement were
Setting Time–Initial (Min.) 108 151 divided into two groups. One group was cured in the fog room (22°C
False Set % 72 ... 100% R.H.) for 70 days after casting and then immersed in a room
Autoclave Expansion % 0.11 0.10 temperature bath of solution containing 50g/L (0.352 moles/L) of
Sulfate Resistance % ... 0.022
Compressive Strength at 1 Day Mpa 15.9 ... Na2SO4 (ASTM C1012-95). The other group was precured in the
Compressive Strength at 3 Days Mpa 27.5 27.4 fog room for 3 days after casting and then placed in a water bath at
Compressive Strength at 7 Days Mpa 33.9 34.1 40°C. Then, 70 days after casting, that group of prisms was trans-
Compressive Strength at 28 Days Mpa 43.3 43.1 ferred into the solution of Na2SO4. The concrete prisms made with
Type 10 cement, Type 10 plus fly ash, and Type 50 cement were pre-
conditioned for 7 days in the fog room and then immersed in the
concrete—the normal material of construction—rather room temperature bath of Na2SO4 solution (Table 2).
than mortar. The point has been made by others that at The concrete cylinders made with high alumina cement were di-
least some tests of concrete itself are desirable to assure vided into groups. One group was cured continuously in the fog
satisfactory performance (Struble et al., 2001). room for about 18 months but 70 days after casting half of that
(b) Would the performance of “modern” high alumina ce- group was immersed in the room temperature bath of sodium sul-
ment differ from that of the material described in the fate solution. Another group was precured in the fog room for only
literature? 3 days after casting and then transferred to a water bath at 40°C for
5. The primary objectives were to use the results of this work in about 18 months. Half the cylinders of that group were transferred,
teaching 3rd and 4th year materials courses. However, the at an age of 70 days after casting, to the room temperature bath of
write-up was amplified to include a brief review of the state sodium sulfate solution.
GILLOTT AND QUINN ON STRENGTH AND SULFATE RESISTANCE 23

FIG. 1—Effect of Na2SO4 Solution on Concrete Prisms.

Concrete cylinders were also made with each of the other three days after casting (Fig.1b). In contrast the prisms placed in
cementitious binders (Type 10 Portland cement; Type 10 plus fly water at 40°C for 70 days prior to immersion in the sulfate
ash; Type 50 Portland cement). In each case some cylinders were bath expanded by 0.025% by 265 days after casting and
held under fog room conditions throughout the test period (18 showed excessive expansion (0.25%) with severe cracking
months) while half of each set was removed from the fog room and deterioration by 433 days (Fig. 1c).
after 7 days and placed in the room temperature bath of sodium 2. The concrete prisms made with the other cementitious agents
sulfate solution (Table 2). showed no significant expansion or cracking during 18
months in the Na2SO4 solution (Fig.1d, e, f ). Expansion val-
Results ues at 18 months for prisms made with Type 10 cement, Type
10 plus fly ash and Type 50 cement were 0.006%, 0.008%,
1. The length change recorded on the concrete prisms made and 0.003% respectively.
with high alumina cement and cured in the fog room for 70 3. Concrete cylinders made with high alumina cement and cured
days prior to immersion in the sulfate bath showed only a in the fog room gained strength rapidly and reached over
very small expansion (0.02%) and no visible cracks by 433 50MPa within 5 days and about 65MPa within 14 days. By 8
24 CEMENT, CONCRETE, AND AGGREGATES

months and 1 year strengths were lower (about 50MPa) but about 1 year. By 18 months the strength had decreased to only
by 18 months some strength recovery to about 60MPa had about 20MPa and the cylinders were cracked and disintegrat-
occurred. ing (Fig. 2c).
4. HAC concrete cylinders placed in the sulfate bath after 7. Concrete cylinders made with Type 10 and Type 50 Portland
70 days in the fog room also had a strength of about cement gained strength more rapidly than the cylinders made
60MPa by 18 months and were generally in excellent with the Type 10 plus fly ash binder but by 28 days all three
condition but a few small cracks were visible in one cylinder types of concrete had compressive strengths in excess of
(Figs. 2a, b). 40MPa. At an age of about 18 months the compressive
5. Concrete cylinders made with high alumina cement and strength of all cylinders was about 55MPa regardless of the
placed in the 40°C water bath after 3 days in the fog room storage conditions. Hence in these tests concrete cylinders
showed a rapid decrease in strength to about 40MPa, which made with the three types of Portland cementitious material
declined further to slightly more than 30MPa at 8 months and and immersed in the Na2SO4 solution had virtually no differ-
1 year with recovery to about 40 MPa by 18 months. ence in compressive strength from that of the cylinders stored
6. The corresponding HAC cylinders placed in the sulfate bath continuously in the fog room and no cracks were visible
after 70 days at 40°C had a strength of a little over 30MPa at (Figs. 2d, e, f ).

FIG. 2—Effect of Na2SO4 Solution on Concrete Cylinders.


GILLOTT AND QUINN ON STRENGTH AND SULFATE RESISTANCE 25

Discussion cylinders, some strength recovery occurred at about 18 months.


Strength recovery has been noted in the literature and attributed by
Sulfates occur in ground water, soils, sea water, fertilizers, and some to growth of hydration products from previously unreacted
industrial pollutants and also form by oxidation of sulfides. When cement. It has also been pointed out that if this is the correct expla-
present in significant amounts they have long been a recognized nation some of the strength recovered may be subsequently lost due
cause of durability failure of Portland cement concrete. More to later conversion. It is possible, however, that strength recovery
recently sulfates have been associated with internal causes of dura- may result from other causes such as a decrease in stress concen-
bility problems such as delayed ettringite formation and thaumasite trations associated with blunting or shortening of small cracks or
attack (Parker, 2000; Gillott & Rogers, 2003; Day, 1992; Collepardi from stress relaxation due to creep and microstructural changes.
1999). In an attempt to address the sulfate problem Bied (1926) de- The HAC concrete cylinders cured in the fog room showed good
veloped high alumina cement, which was patented by Ciments La- resistance to sulfate attack though small cracks were noted in one
farge in 1908 in France following earlier work and patents in Ger- cylinder by about 18 months.
many and England. The cylinders placed in the 40°C bath prior to immersion in the
High alumina cement (calcium aluminate cement, ciment fondu) sulfate solution showed severe cracking and deterioration by an age
is made in a kiln by the fusion of bauxite and limestone with of about 18 months (Figs. 2b, c). These results for the HAC con-
some compounds of iron, which acts as a flux. The principal min- crete prisms and cylinders agree with previous findings reported in
erals formed in the kiln are CA (CaO.Al2O3) and C12A7 the literature which have attributed strength loss and increased
(12CaO.7Al2O3). The material formed in the kiln is ground to a susceptibility to sulfate attack to acceleration of the conversion
fine powder which when mixed with water to a paste hardens and reaction by elevated temperatures in the presence of moisture. This
gains strength rapidly with considerable evolution of heat. Strength conclusion could not be confirmed in this work as neither thermal
may reach 80 per cent of ultimate within 24 hours. On hydration, nor X-ray diffraction data were available.
pseudo–hexagonal calcium aluminum hydrates (CAH10, C2AH8) Sulfates occur in soils in many parts of Canada such as the
and aqueous alumina gel (AH3) are formed. Unlike hydrated Port- Prairie Provinces and Canadian researchers, together with their
land cement Ca(OH)2 is not present in the hydrated paste of high colleagues in the U.S.A. and Europe made early contributions to
alumina cement. The hexagonal Ca–aluminum hydrates are the understanding and remediation of the sulfate problem (Bates
metastable and with time in the presence of moisture they trans- et al., 1913; Mackenzie, 1920; Thorvaldson et al., 1927). The
form to the denser C3AH6 (hydrogarnet) and alumina gel. The recognition of the part played by the individual cement minerals
transformation takes place by a through solution mechanism so wa- paved the way to the development of sulfate resistant Portland ce-
ter has to be present for the reaction to occur. ment and provided a logical explanation for the role of pozzolans
This transformation is known as the conversion reaction, which in improving resistance of Portland cement concrete to sulfate at-
occurs more rapidly with increase of temperature and concentra- tack. The principal cementitious phases in Portland cement paste
tion of lime and alkalies, which is why contact with Portland ce- are calcium silicate hydrates (C-S-H) but Ca(OH)2 and calcium
ment concrete may accelerate conversion. The increase in density sulphoaluminate hydrates are also present. The latter compounds
of the individual crystallites on conversion causes an increase in have been shown to be the most readily attacked by SO4 ions
porosity and permeability and a significant decrease in strength of though C-S-H itself becomes unstable under some conditions so
the cementitious material. Prior to conversion high alumina cement the cement may lose its cementitious properties and all that re-
concrete has excellent resistance to sulfate attack attributed in part mains of the concrete may be aggregates with little or no bond be-
to the absence of Ca (OH)2, to the presence of aqueous alumina gel tween the particles.
and to the low reactivity of CAH10 with sulfate ions. After conver- Resistance of Portland cement concrete to sulfate attack may be
sion however the increased permeability renders the material much improved by reducing the content of Ca(OH)2 and calcium
more liable to poor durability performance since aggressive ions sulphoaluminate hydrates in the cement paste. One approach is to
such as SO3 and CO2 may enter via the pore system. Also sulfate is decrease the ratio of C3S to C2S in the Portland cement since on
said to react expansively with C3AH6 and if CO2 is present it may hydration C3S produces three times as much Ca(OH)2 as is
lead to formation of calcium carbonate (Neville, 1997, p.101). formed by hydration of the C2S. Alternatively pozzolanic materi-
Strength loss attributed to conversion has been considered to be the als such as fly ash or silica fume may be incorporated in the con-
cause of actual structural collapse in various countries. In other crete mixture. Under favorable conditions of hydration those ma-
applications high alumina cement has excellent refractory proper- terials react with the Ca(OH)2 forming C-S-H so a sulfate
ties. There are various descriptions of its nature and behavior susceptible compound with poor cementitious properties is re-
in standard texts (Neville, 1997; Neville and Wainwright, 1975; placed by a more resistant and better bonding agent. The amount
Robson, 1962). of calcium sulpho-aluminate hydrates in the cement paste may be
In the present work the concrete prisms made with high alumina reduced by decreasing the quantity of C3A in the Portland ce-
cement and cured in the fog room prior to being placed in the ment. This is achieved by suitable adjustments to the composition
Na2SO4 bath showed virtually no expansion, cracking or other of the charge entering the kiln during manufacture of the Portland
signs of deterioration to an age of about 18 months (Fig. 1b). cement. In sulfate resistant cement (e.g., CSA Type 50) both the
The prisms immersed in a water bath at 40°C, however, showed C3S to C2S ratio and the C3A content are lower than in Normal
greatly increased susceptibility to sulfate attack since expansion Type 10 Portland cement.
and cracking occurred in the Na2SO4 bath (Fig. 1c). As stated in the section of this paper dealing with the three types
The fog-room cured HAC cylinders showed rapid strength of Portland cement concrete tested none of the prisms showed any
development though strength–loss occurred at an age of about 1 marked change in length during approximately 18 months in the
year followed by strength recovery at a greater age. Immersion in a bath of Na2SO4 solution. Likewise compressive strengths of the
water bath at 40°C, however, led to considerable loss of strength concrete cylinders made with all three types of Portland cementi-
presumably due to conversion though, as with the fog-room cured tious binders exceeded 50MPa regardless of whether conditioned
26 CEMENT, CONCRETE, AND AGGREGATES

in the fog-room or immersed in the bath of Na2SO4 solution. These change in concentration, composition or temperature of the solu-
results indicate that the concrete made here under laboratory con- tion may be better alternatives. It is also possible that continuously
ditions has very satisfactory properties, which may well be superior circulating the Na2SO4 solution may increase its effectiveness by
to that sometimes encountered in the field. Also concrete used in reducing the likelihood that conditions of local equilibrium are
practice is generally subjected to more severe and variable condi- established.
tions of exposure which no doubt affects performance. One of the Concrete made with high alumina cement and cured in the fog
reviewers of this paper suggested that another “aspect to consider room gained strength rapidly and reached higher strength values
is the small specific surface of concrete specimens relative to (65MPa at 28 days) than any of the Portland cement concretes
mortar-bar specimens.” tested (40–45 MPa at 28 days). However the high alumina ce-
It is also possible that the excellent performance of all varieties ment concrete showed a rapid loss of strength and poor resistance
of Portland cement concrete, including that made with Type 10 to sulfate attack after exposure to conditions favoring the conver-
cement, was influenced by the smaller volume ratio of solution to sion reaction. Hence these results appear to support those who
solid than is recommended in ASTM C1012-95. Since this paper consider it prudent to avoid the use of high alumina cement partic-
was submitted for publication additional cylinders (4 in.  8 in.; ularly for structural applications in civil engineering practice
100  200 mm) have been cast using the same mix design as in (Neville, 1998). The close parallel between the performance of this
the previous work but made only with Type 10 Portland cement. “modern” high alumina cement and that reported in previous liter-
About 1/3 of the cylinders are being held under fog-room condi- ature was disappointing since I had nurtured the hope that changes
tions while about 2/3 of the cylinders were removed from the fog- may have been made to this material, which would overcome or
room after 7 days and divided into two sets of 1/3 each. One set moderate its reported drawbacks.
was placed in a room temperature bath (bath #1) of sodium sul-
fate solution (concentration 50 g/L) in which the volume of solu- Acknowledgments
tion was about twice the volume of the concrete cylinders i.e., the
same as in the original work. The second set of cylinders removed Sincere thanks are expressed to Don McCullough and Gerd
from the fog-room was placed in a room temperature bath (bath Birkle for help with the photography and to Chrissy Ziegler for sec-
#2) of sodium sulfate solution (concentration 50g/L) but in which retarial support. Rick Ketcheson, Canada Cement Lafarge, is
the volume of solution was about four times the volume of the thanked for his interest in the work and for the supply of the
concrete cylinders as recommended by ASTM C1012. At an age cements used in the project. Lafarge Canada, Inc. is also thanked
of 90 days the average compressive strength of the cylinders was for the average chemical and physical analyses of the cements.
51.6MPa (fog-room), 49.7MPa (sulfate bath #1) and 48.1MPa
(sulfate bath #2) and no cracks were visible in any of the speci- References
mens. Hence it seems unlikely that the lower volume ratio of so- ASTM C1012-95, 1996, “Standard Test Method for Length
lution to solid than is recommended by ASTM C1012 is the fac- Change of Hydraulic-Cement Mortars Exposed to a Sulfate
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attack. Lime; Gypsum, Vol.04.01, pp. 460–464.
ASTM C642-97.2000, “Standard Test Method for Density,
Conclusions Absorption and Voids in Hardened Concrete,” Annual
Book of ASTM Standards, Concrete and Aggregates,
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appearance, length change characteristics or compressive strength Salts in Alkali Water and Sea Water on Cements,” U.S.
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GILLOTT AND QUINN ON STRENGTH AND SULFATE RESISTANCE 27

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