Scott M.
Schlorholtz 1
Soundness Characteristics of Portland Cement-Fly Ash Mixtures
REFERENCE: Schlorholtz, S. M., ‘‘Soundness Characteristics of
Portland Cement-Fly Ash Mixtures,’’ Cement, Concrete, and Aggre-
gates, CCAGDP, Vol. 20, No. 1, June 1998, pp. 186–191.
ABSTRACT: The Materials Analysis and Research Laboratory has
been monitoring the soundness of several sources of fly ash since the
early 1980’s. The soundness tests were generally conducted in accor-
dance with ASTM Test Method C 311 (the autoclave expansion test
utilizing 20% fly ash and 80% portland cement, specimens prepared
at normal consistency). To date, several thousand tests have been per-
formed on various samples of fly ash that were submitted to the labora-
tory. Also, additional studies were conducted to investigate the
influence of water content (W/CM ratio) and curing regime on the
volume stability of portland cement pastes containing a fly ash that
exhibited soundness problems.
KEYWORDS: fly ash, mineral admixture, portland cement, autoclave
expansion, soundness
Volume stability is an important property of portland cement
concrete. Many different deterioration mechanisms may influence
the volume stability of concrete; however, this paper will restrict
discussion to experiments aimed at evaluating the soundness of
portland cement-fly ash mixtures. In this paper, the term ‘‘sound-
ness’’ implies that a test specimen does not exhibit external dis-
tress, like cracking or flaking, and that it is also free of internal
stresses that may build up and cause excessive expansion over long
periods of time (that is, years).
The major focus of this paper is to summarize the historical
information pertaining to the autoclave expansion of the portland
cement-fly ash mixtures that have been tested at the Materials
Analysis and Research Laboratory (MARL). However, efforts will
also be made to compare and contrast how the autoclave expansion
test results relate to the observed volume stability of pastes cured
for extended periods of time at ambient temperature and pressure.
Comments will also be directed at illustrating how simple changes
in the autoclave expansion calculations can give a better estimate
of how the fly ash influences the test results.
Historically, soundness testing has been conducted on neat paste
specimens that have been prepared at normal consistency. Many
studies have been conducted and repeated attempts have been made
to correlate the basic chemistry (or more specifically, mineralogy)
of cements with the observed test response (ASTM 1936; Gonner-
man et al. 1953; Mehta 1978). The test response that is most com-
monly measured is the linear expansion of prismatic specimens;
however, many different test methods (both quantitative and quali-
tative) have been developed to detect potential soundness prob-
1
Scientist, Iowa State University, Materials Analysis and Research Lab-
oratory, Room 46 Town, Ames, IA 50011.
186
www.astm.org
Copyright by ASTM Int'l (all rights reserved); Wed Mar 9 04:13:14 EST 2011
Downloaded/printed by
Univ Politec Cat-Biblioteca pursuant to License Agreement. No further reproductions authorized.
lems. Also, test specimens have been subjected to many different
treatments in an effort to decrease the time required to identify
unsound specimens. Typical testing environments that have been
used are summarized in Table 1.
After some early controversy on the factors that influenced the
soundness of cements (Erdahl 1920; Blank 1935), it has been estab-
lished that free lime (CaO), periclase (MgO), and tricalcium alumi-
nate (Ca3 Al2 O6 ) dominate the soundness properties of portland
cement (ASTM 1936; Blank 1935; Young 1937; Gonnerman et
al. 1953). Recent research with fly ashes has yielded similar con-
clusions (Schlorholtz 1983; Schlorholtz and Demirel 1985; McCar-
thy et al. 1988).
Experimental Techniques
Description of Analytical Equipment
All chemical assays were performed on a Siemens SRS 200
sequential X-ray fluorescence (XRF) spectrometer. The spectrom-
eter was equipped with a ten-position controlled atmosphere sam-
ple chamber. All specimen measurements were made using a
chromium anode X-ray tube that was operated at 50 kV and 50
mA. The sample chamber was maintained in vacuum mode (27
Pa) throughout the study. The specimens were presented to the
spectrometer as pressed pellets from 1983 until 1987, and as fused
discs from 1987 through the present.
Diffraction experiments were performed on a Siemens D 500
X-ray diffractometer. All specimen measurements were obtained
using a copper anode X-ray tube that was operated at 50 kV and
27 mA. The system was equipped with a graphite monochromator
and a pulse height analyzer. All specimens were presented to the
diffractometer as side-loaded or back-loaded powders. Semi-con-
ductor grade Si metal was used as an internal standard.
Description of Soundness Testing Methods and Equipment
The procedure defined in the ASTM Test Method for the Auto-
clave Expansion of Cement (C 151) was used to conduct the auto-
clave tests. A CENCO autoclave was used throughout this study.
The mix proportions were generally as specified in the ASTM Test
Method for Sampling and Testing Fly Ash or Natural Pozzolans
for Use as a Mineral Admixture in Portland-Cement Concrete (C
311). However, for the purpose of illustration, several of the
aspects of the procedure and mix proportions have been varied in
this study. First, the fly ash content of specific test specimens was
increased above 20% (by mass of cement) to produce soundness
failures in the autoclave. Also, companion specimens of these test
mixtures were subjected to water curing at ambient pressure and
q 1998 by the American Society for Testing and Materials
 SCHLORHOLTZ ON PORTLAND CEMENT-FLY ASH MIXTURES
temperature, to illustrate how the results compare to those obtained
from autoclave curing. Finally, the W/CM ratio of specific mixes
was varied to produce test specimens at consistencies drastically
different than those normally used in the test (that is, normal consis-
tency).
Results and Discussion
Historical Information from the MARL Database
Since 1983 the MARL has measured the autoclave expansion
of several thousand test specimens containing fly ash. Most of the
fly ash samples were obtained from five different power stations
located in Iowa. However, to date, fly ashes from about 60 different
power stations have been tested. The autoclave expansion test
results plus related chemical and physical properties have been
archived in a data base that now summarizes information from
more than 5000 fly ash samples.
A summary of the test results pertaining to soundness is given
in Table 2. The fact that few of the power stations produced fly
ashes that exhibited soundness failures (that is, defined as an auto-
clave expansion greater than 0.8%) reinforces the validity of recent
changes in the sampling and testing frequency suggested in ASTM
C 311. Typically, soundness problems appear to be linked to fly
ash obtained from specific power plants, rather than appearing
sporadically in all fly ashes. However, be aware that this observa-
tion needs to be tempered by the fact that the information (Table
2) reflects only a single level of fly ash replacement (20% by mass
of cement).
There are a few difficulties that are encountered when one is
attempting to evaluate the soundness of portland cement-fly ash
mixtures. This is especially true when the evaluation spans across
many years.
First, one must keep in mind that the portland cement chosen
for use in any given laboratory has an influence on the expansion
observed in the autoclave test. However, the real reason for per-
forming the test on any given fly ash is to evaluate how the fly
TABLE 1—Typical test methods used to evaluate soundness.
Temperature and Duration of Test,
Type of Test Pressure approximate
Water cure 21 to 248C ambient months to years
pressure
Storage over 1008C ambient pressure varied from 5 to 24 h
boiling water
Le Chatelier test 1008C ambient pressure 1h
Autoclave (early 1758C varied from 1 to 3 days
187
influences the test response. Hence, Example 1, which follows,
gives a rough method that helps to remove much of the expansion
that was caused by portland cement. The correction method is
based on the principal of superposition; and hence, is offered only
as a first approximation to the expansion that was produced exclu-
sively by the fly ash.
Secondly, it is important to note that the current test method
uses a fixed percentage of fly ash (20% by mass of cement); and
this may lead to a false sense of security in some instances. This
concept will be discussed later in Example 2, which illustrates a
classic case of unsoundness caused by a problematic fly ash. The
concern here is not that unsound fly ashes could be incorporated
into any given product because the current specification protects
users via the existing physical requirements (for example, refer to
Note C in Table 2 of ASTM C 618). Rather, the concern is based
on our limited ability (due to the ‘‘standard’’ 20% replacement)
to define sources of fly ash that may at some arbitrary time produce
fly ashes that are unsound. Previous research has illustrated that
some portland cement-fly ash mixtures tend to become unsound
over very narrow ranges of fly ash concentration. This has been
the case over the many years that this author has studied soundness
(Schlorholtz 1983; Schlorholtz and Demirel 1985).
Example 1: Removal of Cement Expansion from the Test
Response
Autoclave expansion tests are normally conducted on specimens
that contain 80% portland cement and 20% fly ash, and have been
proportioned with enough water to reach a consistency denoted as
‘‘normal consistency.’’ Both cements and fly ashes can contain
expansive constituents (that is, free lime, periclase, and tricalcium
aluminate) that contribute to the overall measured expansion of
the test specimen. However, it is often desirable to know how
much of the expansion can be attributed to changes in the fly ash.
The procedure that has been used at this laboratory consists of
subtracting the expansion of a control specimen of the cement from
the expansion that was observed for the test specimen containing
both cement and fly ash. The expansion of the control specimen
is normally corrected for the level of fly ash replacement (that is,
0.8 times the cement expansion for standard tests). This concept
is best illustrated by the following example.
Our laboratory had just depleted its supply of Cement A and
had changed to a new (fresh) one, which will be referred to as
Cement B. Nearly immediately, the fly ash marketing agency
called and asked why the autoclave expansion test results had
increased so dramatically. Hence, a series of 20 consecutive sam-
188 CEMENT, CONCRETE, AND AGGREGATES

TABLE 3—Composition of cements and fly ashes used in Example 1.

Fly Ash 1–5 Fly Ash 6–10 Fly Ash 11–15 Fly Ash 16–20
 SCHLORHOLTZ ON PORTLAND CEMENT-FLY ASH MIXTURES 189

FIG. 2—Autoclave expansion of test specimens containing various percentages of fly ash from Power Plant F.

FIG. 3—X-ray diffractogram of fly ash from Power Plant F.

Copyright by ASTM Int'l (all rights reserved); Wed Mar 9 04:13:14 EST 2011
Downloaded/printed by
Univ Politec Cat-Biblioteca pursuant to License Agreement. No further reproductions authorized.
190 CEMENT, CONCRETE, AND AGGREGATES

The influence of W/CM ratio was also studied because many
Class C fly ashes tend to reduce the amount of mixing water
that is required to reach normal consistency. Keep in mind
that the autoclave specimens are generally molded at equivalent
consistencies (normal consistency), rather than equivalent water
contents. This poses a dilemma because soundness tests are
conducted to evaluate the slow (or delayed) hydration of expan-
sive components; however, the expansive components cannot
hydrate if they do not have sufficient water. How much water
is sufficient? This is a difficult question to answer quantitatively;
however, a few test specimens were molded at various water
contents to see if this variable was critical to soundness failures
in the autoclave test.
Figure 4 depicts the influence of fly ash content on the W/CM
ratio needed to produce portland cement-fly ash pastes at normal
consistency. As mentioned earlier, the Class C fly ash reduced the
amount of water needed to reach normal consistency. However,
varying the water content of the test specimens containing 30 and
40%, respectively, of the unsound fly ash had little influence on
the outcome of the autoclave expansion tests (Table 5). Again,
the expansions summarized in Table 5 should only be considered
qualitatively because of the difficulty encountered when attempting
to measure specimens that exhibit such severe distortion; however,
failure was plainly evident in each of the test specimens. The speci-
mens denoted as ‘‘very wet’’ in Table 5 were so fluid that they
had to be poured into the autoclave bar molds. Hence, there was
plenty of free water available to hydrate the various constituents
of the paste.
In this study, the autoclave test results obtained using fly ash
from Power Plant F were only in qualitative agreement with com-
panion test specimens that had been cured at ambient pressure and
temperature (Fig. 5). These test specimens, which contained 20 to
40% of the problematic fly ash, were molded and cured using the
normal procedure. Then they were immersed in a water bath at
room temperature, rather than being subjected to the normal auto-
clave curing cycle.
The test specimens exhibited rapid expansion during the first
few days of curing. This was followed by a substantial decrease
in the rate of expansion (days 7 through 90), and finally, after
approximately three months of curing, the expansion stopped. The
test specimens are still being monitored periodically to assess their
long-term stability.
As mentioned above, the results of the autoclave tests were only
in qualitative agreement with the tests that were conducted at ambi-
ent temperature and pressure. In general, both the autoclaved and
water-cured specimens exhibited increasing expansion with
increasing levels of fly ash replacement. However, only the speci-
mens containing 20% fly ash expanded similar amounts (0.12%
in the autoclave and 0.11% after six months in the water bath).
The portland cement control specimen expanded nearly three times
more in the water bath than it did in the autoclave. The test speci-
mens that failed miserably in the autoclave (that is, containing 30
and 40% fly ash), expanded less than 0.2% after six months in the
water bath. Of course, there is no valid reason to assume that the
test specimens in the water bath have totally stopped expanding,
only time and continued monitoring will establish their true sound-
ness characteristics. However, if the influence of the portland
cement is removed from the test response (Fig. 6), then the expan-
sion curves appear to be very flat, with little indication of impend-
ing failure.

FIG. 4—Influence of fly ash content on the amount of water needed to

produce test specimens at normal consistency.

TABLE 5—Influence of varying the water content of test specimens on

the results of the autoclave expansion tests.
Description of Test Fly Ash Content, W/CM Expansion,
Specimen mass % Ratio %

Control cement, at 0 0.262 0.03

normal consistency
30% fly ash, at normal 30 0.236 4.9 (failure)
consistency
30% fly ash, at wet 30 0.242 5.8 (failure)
consistency
30% fly ash, at very wet 30 0.248 4.9 (failure)
consistency
40% fly ash, at normal 40 0.230 8.4 (failure)
consistency
40% fly ash, at wet 40 0.236 8.4 (failure)
consistency
40% fly ash, at very wet 40 0.242 8.4 (failure)
consistency FIG. 5—Paste expansion versus time for the test specimens cured at
ambient pressure and temperature.

Copyright by ASTM Int'l (all rights reserved); Wed Mar 9 04:13:14 EST 2011
Downloaded/printed by
Univ Politec Cat-Biblioteca pursuant to License Agreement. No further reproductions authorized.
 SCHLORHOLTZ ON PORTLAND CEMENT-FLY ASH MIXTURES
FIG. 6—Corrected expansion versus time for the test specimens con-
taining various amounts of fly ash.
Summary
In summary, this paper has attempted to show how fly ash can
influence the soundness of portland cement-fly ash pastes. It is
important to realize that fly ash often contains free lime, periclase,
and tricalcium aluminate, and that these are the same compounds
that have been attributed to unsound behavior in portland cements.
These constituents function much the same way in fly ash; how-
ever, little attempt has been made to quantify these minerals.
Copyright by ASTM Int'l (all rights reserved); Wed Mar 9 04:13:14 EST 2011
Downloaded/printed by
Univ Politec Cat-Biblioteca pursuant to License Agreement. No further reproductions authorized.
191
Instead, the autoclave expansion test has been used to provide a
performance criterion that all fly ashes must meet. This appears
to be conservative in most instances because the autoclave test is
so sensitive to the presence of free lime; however, it also fails to
contribute to our knowledge concerning the fundamental mecha-
nisms that produce unsound behavior.
References
American Society for Testing and Materials, 1937, ‘‘Report of Working
Committee on Volume Change and Soundness of Portland
Cement,’’ Proceedings of the 39th Annual Meeting of ASTM, Vol.
36, Part 1, Committee Reports, pp. 225–251.
Blank, A. J., June 1935, ‘‘Causes of Unsoundness of Cement,’’ Concrete-
Cement Mill Section, Vol. 43, No. 6, pp. 38–40.
Erdhal, B. F., June 1920, ‘‘Cause of Unsoundness in Portland Cement,’’
Concrete-Cement Mill Section, Vol. 16, No. 6, pp. 133–135.
Gonnerman, H. F., Lerch, W., and Whiteside, T. M., June 1953, PCA
Laboratory Bulletin 45.
McCarthy, G. J., Solem, J. K., Manz, O. E., and Hassett, D. J., 1988, ‘‘Use
of a Database of Chemical, Mineralogical and Physical Properties
of North American Fly Ash to Study the Nature of Fly Ash and
Its Utilization as a Mineral Admixture in Concrete,’’ Materials
Research Society Proceedings, Vol. 178, Materials Research Soci-
ety, Pittsburgh, pp. 3–33.
Mehta, P. K., 1978, ‘‘History and Status of Performance Tests for Evalua-
tion of Soundness of Cements,’’ ASTM STP 663, American Society
for Testing and Materials, West Conshohocken, PA.
Schlorholtz, S., 1983, Autoclave Expansion of Portland Cement-Fly Ash
Pastes, MS Thesis, Iowa State University.
Schlorholtz, S. and Demirel, T., 1985, ‘‘Autoclave Expansion of Portland
Cement Fly Ash Pastes,’’ Materials Research Society Symposium,
Vol. 43, Materials Research Society, Pittsburgh, pp. 85–93.
Young, R. N., Sept.–Oct. 1937, ‘‘The Autoclave Test and Interpretations,’’
Journal of the American Concrete Institute, Vol. 34, pp. 13–22.