Gaurav Paper On Shrinkage Measurement

Sant, Lura, and Weiss Measurement of Volume Change in Cementitious Materials at Early Ages Page 1 of 19
Measurement of Volume Change in Cementitious Materials at Early Ages:

Review of Testing Protocols and Interpretation of Results
Gaurav Sant
Undergraduate Research Assistant
School of Civil Engineering
Purdue University
West Lafayette, IN 47907-1284
Email: gsant@purdue.edu
Phone: 765-494-5025
Fax: 765-496-1364
Pietro Lura
Assistant Professor
BYG DTU - Department Civil Engineering
Technical University of Denmark
Brovej, DTU - Building 118
2800 Kgs. Lyngby
Denmark
Email: plu@byg.dtu.dk
Phone: +45 45 25 17 58
Fax: +45 45 88 32 82
Jason Weiss (Corresponding Author)

Associate Professor and Assistant Head for Research
Associate Director of the Center for Advanced Cement Based Materials
School of Civil Engineering
Purdue University
West Lafayette, IN 47907-1284
Email: wjweiss@purdue.edu
Phone: 765-494-2215
Fax: 765-496-1364
Number of Words: Abstract 203, Body 5515, 7 Figures 1750 = Total 7468
Submitted to the Transportation Research Board for possible presentation and publication
Date of Original Submission: July 30, 2005, Date of Final Submission: November 14, 2005
TRB 2006 Annual Meeting CD-ROM Paper revised from original submittal.
Measurement of Volume Change in Cementitious Materials at Early Ages:

Review of Testing Protocols and Interpretation of Results
Gaurav Sant, Pietro Lura, and Jason Weiss
ABSTRACT
Early-age cracking in concrete bridge decks, pavements, and superstructure elements has served
as the impetus for substantial research on early-age shrinkage in cementitious materials over the
last two decades. Much of this research has indicated how mixture proportions, constituent
materials, and construction operations can be altered to reduce the risk of cracking.
Unfortunately, many unrestrained shrinkage-testing protocols do not provide a comprehensive
picture of the early-age shrinkage exhibited by cementitious materials, especially those used in
higher strength concrete. In this paper, the authors review several early-age shrinkage testing
procedures. A testing protocol is presented to show how chemical shrinkage can be measured
using buoyancy measurements. A comparison of the measured autogenous shrinkage is made
using four measurement methods: a sealed membrane, a corrugated tube, a non-contact
measurement in a rigid mold, and the ASTM C157 standard. The results of the autogenous and
chemical shrinkage tests are compared with one another to fully describe early-age length
change. It is shown that through careful experimentation and interpretation, the results of these
tests can be completely correlated with one another. This can provide the end-user with reliable
test procedures to compare different paste compositions, different admixtures, and provides
inputs for models that quantify the cracking potential.
1.0 BACKGROUND
Over the last two decades, substantial research has been devoted to studying the
susceptibility of concrete to early-age cracking. The abundance of research on early-age
cracking has lead to a better understanding of the role of mixture proportions and to the
development of early-age* cracking simulation models [1,2]. Unfortunately however, shrinkage
measurements may not always be performed in a comprehensive manner. For example, Aïtcin
[3] illustrated that, while the standard ASTM procedure (C157 [4]) may be satisfactory for
measuring free shrinkage in high water-to-cement ratio (w/c) mixtures, difficulties arise when
this method is ‘blindly extended’ to low w/c mixtures†. These difficulties can be traced to the
self-desiccation of the cement paste which causes autogenous shrinkage during the first 24 hours,
before the concrete is demolded and the ASTM C157 measurements are begun. A simple
example of the consequence of not recording this early-age shrinkage is shown in Figure 1. It
can be seen that if the ASTM C157 procedure is followed (on a sealed paste specimen with a w/c
of 0.30) the shrinkage may be measured to be 860 µε‡ at 7 days, while a substantially larger
strain is measured if the measurements are begun 30 minutes after mixing§ (5130 µε at 7 days).
The actual magnitude of shrinkage that is important for describing restrained shrinkage and
cracking potential lies somewhere between these values.
0
Linear Shrinkage (µε)
-1000
ASTM C-157 (Sealed)
-2000 Autogenous Shrinkage
(Corrugated Tube Method)
-3000
-4000
-5000
ASTM C-157 (Sealed) + 24 Hour Offset
-6000
0 24 48 72 96 120 144 168
Age of Specimen (hours)
FIGURE 1 A comparison of the autogenous shrinkage measured in sealed specimens using

the ASTM C157 procedure (beginning at 24 hours) and the corrugated mold procedure
(beginning immediately after mixing) for a w/c = 0.30 mixture
*
In this paper the phrase ‘early-age’ will be used loosely to refer to cement and concrete materials from the time of
mixing through the first seven days at standard room temperature. This is consistent with the definition of ACI 231.
†
‘Low w/c’ in this paper refers to pastes where substantial self-desiccation and autogenous shrinkage may take
place, which is typically a w/c of less than 0.42.
‡
µε will be used throughout this paper. To obtain strain you would multiply µε by 10-6.
§
It should be noted that the linear autogenous shrinkage shown in Figure 1 is obtained directly from the corrugated
mold without any corrections to account for the anisotropic behavior of the corrugated mold before set. The authors
will discuss this aspect of the test in greater detail in section 3.3.2 and indicate how to address anisotropy at that
point.
The primary reason for the differences in total shrinkage determined using the different
test methods is that shrinkage begins immediately as the water comes in contact with the cement,
as observed by Le Chatelier [5] over a century ago. As such, shrinkage tests can be sensitive to
the time at which they start. At this point it is helpful to clearly define two specific types of
shrinkage that will be discussed in this paper: chemical shrinkage and autogenous shrinkage [6].
Chemical shrinkage refers to “the volume reduction associated with the hydration reactions in a
cementitious material [6]” while autogenous strain is “the bulk strain of a closed, isothermal,
cementitious material system not subjected to external forces [6]”. Although autogenous strain
and autogenous shrinkage are synonyms when a net volume reduction occurs, the term
autogenous strain is more general since it enables expansions to also be considered.
While these definitions are relatively straightforward, their physical measurement and
relationship to concrete mixture design and structural analysis can be more difficult. For
example, shrinkage occurring before a rigid skeleton develops in the concrete is of little practical
significance in the problem of early-age cracking, since it does not result in residual tensile
stresses. However, as cementitious materials hydrate they begin to stiffen. The time at which
the fluid-like behavior of the cement paste gives way to a material with a rigid skeleton is
commonly referred to as ‘setting’ and is frequently measured using methods like the pin-
penetration (ASTM C-403M) and the Vicat test (ASTM C-191) [7,8]. The current ASTM tests
are related to the materials resistance to a mechanical pressure and, while simple to perform, they
are somewhat arbitrarily related to the physical structure of the material. While it may be
thought that setting time is somewhat trivial, it can have immense practical significance both for
determining the time to begin shrinkage measurement as well as to determine the time that
should be used for beginning computer simulations [9].
Figure 2 compares the results of chemical and autogenous shrinkage for a paste with a
w/c of 0.30. Initially, both specimens are fluid and the response of both test methods is very
similar. After setting, the shrinkage that is measured in a hardening sealed specimen (i.e., the
autogenous shrinkage) is much less than the chemical shrinkage, since the newly-formed
structure of the cement paste resists the volume change. The difference between the chemical
and autogenous shrinkage has been explained by the development of gas (vapor) filled voids that
form inside the paste [5]. The chemical shrinkage test enables water to enter the system after the
structure is formed (i.e., it is an open system) and measures the total volume change of the
cement paste, included the inner porosity. However the autogenous shrinkage test does not
permit the vapor filled space to be filled with water since it is sealed (i.e., a closed system), and
measures only the external volume change of the sealed cement paste. Although there is
agreement that the chemical and autogenous shrinkage diverge around the time of set, there is a
lack of a consistent standard to measure the response of these materials at early ages [1, 3, 10,
11, 12, 13].
This paper examines different techniques for measuring chemical and autogenous
shrinkage in low w/c pastes at early-ages. Specifically, this paper will:
• Review and compare testing procedures to measure chemical and autogenous shrinkage
in cementitious materials at early ages.
• Discuss the impact of specific features of the chemical shrinkage testing protocol on the
chemical shrinkage results.
• Compare results from four techniques for measuring autogenous shrinkage: the
membrane method, the corrugated tube method, the rigid form method, and ASTM C-
157 on sealed specimens.
• Compare the divergence of chemical and autogenous shrinkage with ‘setting time’ as
measured using the Vicat test.
In addition this paper calls attention to the need for measuring shrinkage at very early ages
and it illustrates precautions that should be taken to acquire repeatable and reliable data of the
shrinkage response of pastes. This can be used to develop new testing protocols that fully
describe shrinkage for use in material comparison, database development, and determination of
model inputs.
0
Autogenous Shrinkage (Membrane Method)
Linear Shrinkage (µε)
-4000
-8000
-12000
-16000
W/C = 0.30 Chemical Shrinkage (Bouyancy Method)

-20000
0 6 12 18 24 30 36 42 48
FIGURE 2 A comparison of the chemical shrinkage (as measured using the buoyancy
method) and autogenous shrinkage (as measured using the membrane method) for a
mixture with a w/c of 0.30. Both chemical shrinkage and volumetric autogenous shrinkage
have been converted into linear shrinkage assuming isotropic deformations (i.e. dividing by
a factor 3). Every 20th data point is shown.
2.0 REVIEW OF TEST METHODS FOR EARLY-AGE SHRINKAGE

Although early age shrinkage has been measured in cementitious systems for over a century
[5], it is common to find a wide range of measurement and interpretation procedures that may
not fully capture all of the shrinkage behavior. The following section will review some of the
more common approaches that have been used to measure chemical and autogenous shrinkage.
In addition, a critical discussion is presented to highlight some aspects of these tests that may
lead to artifacts or irreconcilable results.
2.1 Chemical Shrinkage

Le Chatelier [5] first observed that hydration of cement caused a reduction in the absolute
volume of a cement paste. Early chemical shrinkage results were used to quantify the extent of
chemical reaction that had taken place. For example, Powers [14] used measurements of
chemical shrinkage (i.e., measurements he called absorption) as “an index to the progress of the
reactions”. Knudsen and Geiker [15,16] related chemical shrinkage with compressive strength
development. More recently, researchers have begun to use chemical shrinkage as an indicator
of the extent of autogenous shrinkage that may occur in a concrete [10,11]. While chemical
shrinkage measurements in each of these tests followed similar concepts, it is only within the last
year that a standard testing procedure has been developed in North America for chemical
shrinkage tests [17].
The primary objective of any chemical shrinkage test is to quantify the change in volume
that occurs due to the hydration reactions. The chemical shrinkage is generally quantified by
measuring the amount of water that is sorbed by a saturated cement paste [18].
Two primary test methods have been reported in literature, tests that measure the volume
change of liquid in contact with the cement paste and tests that measure the change in buoyancy
(or weight) of an immersed cement paste specimen in contact with water. The volumetric
method is generally based on the change of water level in a capillary tube above a paste
specimen [16]. While this test method is economical, it is time consuming because the height of
the water needs to be measured at regular intervals; moreover, it is difficult to automate although
methods like the use of a photoelectric cell have been described by Buil [20] and summarized by
Geiker [16]. The second method is based on the change in density/buoyancy that occurs when
water is absorbed in the hydrating specimen. These methods have been described by Rey [19]
and summarized in English by Geiker [16]. This paper will utilize a density/buoyancy
measurement that will be described in greater detail in section 3.1.
It should be noted that, however apparently simple, these test methods have several
experimental difficulties that can result in spurious results. First, the thickness of the specimen
[11, 16] influences the results, since thicker specimens (especially specimens with a low w/c)
develop a low porosity and water can not travel fast enough to fill in the vapor-filled voids
created by chemical shrinkage. In addition, the water on the surface of the specimen could have
a different chemistry than the fluid in the pores, possibly resulting in leaching. Variations in the
sample temperature that occur during hydration may also influence results, especially if the
samples are large. Moreover, the cement pastes used should be deaired, since air bubbles
reaching the surface of the paste and leaving the sample would result in a change of submerged
weight. Some of these effects will be illustrated by experiments in this paper.
2.2 Autogenous Shrinkage

Measurements of autogenous strain have been carried out in two fundamentally different
ways: measurement of volumetric strain and measurement of linear strain. Volumetric
measurements are frequently performed by casting the fresh cement paste in a rubber balloon
that is immersed in a fluid. The volume change of the cement paste is measured for example by
monitoring the weight change (i.e., buoyancy change) of the immersed sample [20]. Linear
measurements are frequently performed by casting the cement paste in a rigid mold with low
friction and recording the length change by a displacement transducer at one end of the specimen
[21].
Both methods have been extensively used in parallel for more than 50 years [22, 23] and
each possesses advantages and disadvantages [6]. One advantage of the volumetric method is
the possibility of starting the measurements immediately after casting; however, the lack of a
steady contact between the rubber membrane and the cement paste is a considerable
disadvantage of the volumetric method. A film of water (e.g., due to bleeding or entrapped air)
at the surface of the cement paste may obstruct this contact significantly. During the hydration
process the water or entrapped air may be sucked back into the cement paste as a consequence of
chemical shrinkage. In this way, the internal volume reduction may be erroneously measured as
an outer deformation. Another major source of error is osmosis through the membrane used in
volumetric measurements [24].
One advantage/disadvantage of the linear method is the need for firm anchorage of the
measuring points to the set cement paste. While this provides a clear indication of length to be
used as the original length, it prevents the measurements to be started before the cement paste
has set [25]. An additional problem is the risk of restraining the cement paste, especially in the
very first hours after setting. At early-ages the cement paste may be too weak to overcome the
friction against a rigid mold; however this problem can be reduced by lubricating the mold.
Bleeding may also influence the linear measurement of autogenous strain. After setting, the
bleed water may be reabsorbed by the cement paste and reduce the autogenous shrinkage or even
cause expansion [11].
Jensen and Hansen [26] developed a special, corrugated mold system, which combines
the advantages of linear and volumetric measurement of autogenous strain. Before set, the lack
of longitudinal stiffness of the corrugated mold transforms the volumetric strain into a linear
strain, and after set a normal, linear strain is measured. In this way, it is possible to start linear
measurements directly after casting.
3.0 EXPERIMENTAL PROTOCOLS USED IN THIS STUDY
3.1 Chemical Shrinkage – Buoyancy Protocol

Measurement of chemical shrinkage on cement pastes was performed in this study by
monitoring the change in buoyancy that occurs for samples suspended in paraffin oil. The
testing apparatus is illustrated in Figure 3. Each chemical shrinkage test consists of deaired
freshly mixed cement paste (the deairing process is described in detail in section 4) that was
placed in a cylindrical glass crystallization dish (70 mm in diameter and 50 mm tall). While the
weight of the paste in this study was varied to include sample sizes of 25g, 50g, 100g, and 200g
(these sample sizes were based on samples used in earlier studies [11,16)) to illustrate the effect
of specimen size, the 25g sample is the typical sample size used in the typical studies at Purdue.
After the cement paste was placed in the glass crystallization dish the specimens were vibrated
until a uniform amount of paste was spread over the bottom of the dish. The cement paste layer
thickness varied from approximately 3 to 24 mm (depending on the weight of the paste used).
After vibration was complete, a layer of deaired and deionized water (or deaired synthetic pore
solution) was applied to the surface of the paste with an eyedropper until a continuous film of
fluid was formed. For the normal test conditions, 10 grams of water were used, however
different amounts of water (or synthetic pore solution) were employed to demonstrate the effect
of the volume of water. It should be noted that 10 grams of water was chosen for two reasons.
First it would provide sufficient fluid to compensate for the roughly 7% volume change that may
be expected during hydration. Second, it would enable the entire surface of the cement paste to
be covered with water (or the ponding fluid) during the test, since slight changes in balance
could provide a layer of water of varying thickness across the top of the specimen. After the
addition of water to the surface of the paste, paraffin oil was applied drop by drop, until it
covered the entire surface of the water in the beaker. More paraffin oil was added until the
crystallization dish was nearly completely filled.
Balance
Hook
Monofilament
Line
Crystallization
Dish
Paraffin oil
Water
Paraffin
Oil
Water or
Sample Pore
Solution
Paste
Sample
Wire Mesh
Holder
(a) (b)
FIGURE 3 An illustration of experimental procedures to measure chemical shrinkage: a)

an illustration of the buoyancy method and b) a photo of the chemical shrinkage test
specimen
The crystallization dish was positioned on a stainless steel mesh platform that was
suspended with monofilament multi-purpose fishing string lines from a steel hook (Figure 3b).
The hook was connected to a string and suspended from the high-precision balance plate. The
crystallization dish was then gently lowered into a plastic container filled with paraffin oil (i.e.,
the container included approximately 5 liters of paraffin oil). To maintain the sample
temperature constant, the container of paraffin oil was submerged in a temperature regulated
water bath at 23±0.2°C with water circulation, which contained approximately 25 liters of
distilled water. The majority of surface of the bath was covered with an acrylic plastic lid to
reduce evaporation.
The balance sensitivity was 0.1 mg which resulted in a nominal accuracy on the
measured chemical shrinkage of about 2⋅10-6 ml/gcem, considering the typical sample sizes used
in this study. The actual uncertainty on the measurements is approximately 10 times higher,
being dominated by a number of factors, including vibrations in the water bath and uncertainty
on the density of the paraffin oil. The balance was placed on a massive weighing table to
minimize vibrations.
The submerged weight of the sample was recorded automatically every 5 minutes from
the time the specimen was placed in the bath (30 minutes after the addition of water to the dry
cement during mixing). Equation 1 describes how the chemical shrinkage was calculated
∆V paste (t ) Wsub (t ) − Wsub (30 )

VCS = = (1)
g cem ρ par ⋅ g cem
where ∆Vpaste (ml) is the volume change of the paste, gcem (g) is cement content by mass of the
cement paste, Wsub(t) (g) is the submerged weight of the paste at time t, Wsub(30) (g) is the initial
submerged weight of the paste 30 minutes after water addition, and ρpar (g/ml) is the density of
the paraffin oil in the buoyancy bath (i.e., measured to be 850 kg/m3 at 23ºC). Chemical
shrinkage measurements will be generally presented in this paper as volume change per gram of
cement in the mixture (ml/gcem).
3.2 Autogenous Shrinkage Measurement Protocols

Measurements of the autogenous shrinkage of a cement pastes were performed using four
separate approaches: the membrane method, the corrugated tube method, the rigid form method,
and ASTM C-157 on sealed specimens. The following section describes each of the testing
protocols used in this study.
3.2.1 Autogenous Shrinkage – Membrane Method Protocol

The measurement of autogenous strain was performed by monitoring the weight of a
cement paste sample that was sealed in a membrane, submerged in paraffin oil, and suspended
from a high-precision balance. The test setup is shown in Figure 4a. For each test, 100 to 150 g
of deaired, freshly mixed cement paste was cast in a membrane. Lura and Jensen [23] illustrated
the errors that can arise if a specimen absorbs water during the test. As such, the choice was
made to suspend the specimens in paraffin oil and the membranes were carefully screened to
avoid membranes that would absorb water or paraffin oil. The membranes consisted of
polyurethane condoms with thickness 0.04 mm. It should be pointed out that the weight of the
sample should always be monitored before and after the test to determine if liquid from the bath
penetrated the membrane.
Corrugated Data Conditioning

Balance Tube and Acquisition
Threaded
Adjustment Screw
Paraffin oil
Water
Sample
LVDT
Sample Holder
(a) (b)
FIGURE 4 An illustration of experimental procedures to measure autogenous shrinkage:

a) the buoyancy method and b) the corrugated tube method
The membranes were cleaned and any lubricants were removed with a paper towel. After
cleaning, the membranes were filled with cement paste. The filled membrane was tightly closed
with a knot, paying careful attention to avoid the entrapment of air bubbles. The excess part of
the membrane was then cut off and a monofilament line was tied to the sample. The line,
approximately 400 mm long, was tied to a stainless steel hook. The sample was then gently
lowered into a plastic container filled with paraffin oil that was placed in the temperature
regulated water bath described in section 3.1.
The weighing accuracy of the balance results in a nominal accuracy on the measured
strain of 0.5 µε, considering typical sample sizes and isotropic deformations. The actual
uncertainty on the measurements is about 10 times higher, being dominated by a number of
factors, including vibrations induced by the water circulation in the water bath.
The submerged weight of the sample was automatically recorded every 5 minutes from
about 30 minutes after water addition up to a few days. Volumetric strain (εVol) of a cement
paste can be calculated from the submerged weight change according to the following procedure:
∆V paste (t ) Wsub (t ) − Wsub (30)

ε Vol = = (2)
V paste (30 ) ρ par ⋅ V paste (30)
where ∆Vpaste(t) (ml) is the volume change of the paste at time t, Vpaste(30) (ml) is the initial
volume of the paste, Wsub(t) (g) is the submerged weight of the paste at time t, Wsub(30) (g) is the
initial submerged weight of the paste, and ρpar [g/ml] is the density of the paraffin oil in the
buoyancy bath. The initial weight and volume are taken 30 minutes after the addition of water to
the mixer.
Volumetric strain is converted to linear strain (εLin) using equation 3 and assuming
isotropic deformations:
ε Vol
ε Lin = (3)
3
3.2.2 Autogenous Shrinkage – Corrugated Tube Method Protocol

Linear autogenous strain of cement pastes was measured in a technique where the fresh
paste was placed in corrugated polyethylene molds with a length-to-diameter ratio of
approximately 400:30 mm [24]. The technique is designed to encapsulate the fresh cement paste
while minimizing restraint, thereby permitting measurements to start 30 minutes after water
addition. The corrugated mold transforms volumetric deformations into linear deformations
when the paste is in a fluid state since the mold has a greater stiffness in the radial direction than
it does in the longitudinal direction. The ratio between the length and volume change was found
to be 1.85 mm/ml by injecting a known volume of a liquid into the corrugated moulds [27].
Length changes occurring before set should be divided by 2.53 if isotropic deformation is used as
a reference [27]. The corrugated molds were specially designed to minimize restraint on the
paste (less than 0.1 MPa). The molds are also watertight.
The cement paste was cast into the corrugated tube and vibrated. The specimen was then
placed in a dilatometer kept in a room at 23±1°C. The dilatometer was equipped with automatic
data-logging and electronic linear displacement transducers (Figure 4b); the measuring accuracy
was ±5 µm/m. The measurements were performed every 5 minutes and started at about 30
minutes after water addition.
3.2.3 Autogenous Shrinkage – Rigid Form Method Protocol

The third procedure used to measure autogenous shrinkage consists of the use of a non-
contact laser to investigate length change of a specimen in a conventional rigid steel form [28].
The lasers operate on the principle that a laser light beam is projected toward a surface at a small
angle from the perpendicular direction. This laser light beam is reflected back to a sensor and
the distance from the laser head to the surface can be calculated by using Snell’s law. As the
specimen shrinks the path of the reflected beam changes activating a different portion of the
sensor and the distance from the sensor can be calculated [27]. For the experiments described in
this paper, an invar steel mold was used with an inner dimension of 25 mm × 25 mm × 300 mm.
The inner surface of the steel mold was lined with two thin sheets of mylar in order to reduce any
restraint due to bonding. Openings were located at either end of the mold to provide a path for
the laser light beam to pass through the mold and contact the specimen. The inner surface of the
openings was covered with clear, thin plastic film, which stayed in place throughout the test.
The top of the specimens was covered with a 3 mm plastic sheet during the test to prevent
moisture loss.
Two measurements were performed on the samples in the rigid molds. The first
measurement considers the specimen length change (i.e., in the 300 mm direction) while the
second measurement considers the change in specimen height (i.e., in the 25 mm direction).
The lasers were capable of measurements that are accurate to ± 0.1 µm however practical
considerations appear to indicate that an accuracy of ± 5 µm may be more appropriate when
considering all sources of uncertainty. The measurements are recorded every 5 minutes by
taking the average of 10 measurements starting 30 minutes after water was added to the cement
powder.
3.2.4 Autogenous Shrinkage – ASTM C157 Testing Method Protocol – Sealed

The standard ASTM unrestrained length change procedure (ASTM C157) was also
performed. The measurements were begun at an age of 24 hours when the 25 mm x 25 mm x
300 mm specimens were removed from the molds, wrapped in two layers of aluminum tape [29],
and measured in a comparator. The average length change of two specimens is reported for each
measurement.
3.3 Setting Time

To determine the time of setting of the cement pastes the Vicat Test (ASTM C191) [8]
was performed.
4.0 EXPERIMENTAL PROGRAM

This paper describes a series of tests using a paste with a w/c of 0.30. The mixtures
described in this paper have also been prepared in a slightly less conventional manner than those
commonly reported in literature. The pastes were deaired, neat cement pastes to minimize the
influence of air on the buoyancy measurements. As such the pastes were prepared using de-
ionized water that was deaired prior to mixing by boiling it for a few minutes to remove the
dissolved air. A type I portland cement was used with a Blaine fineness of 3470 cm2/g and a
compound composition of 60% C3S, 12% C2S, 12% C3A, and 7% C4AF. The water was cooled
to room temperature prior to mixing. The dry constituent materials were placed inside a special
mixing chamber [30] that was sealed. Air was evacuated from the chamber using a vacuum
pump (to a pressure of 725 mm of Hg for 45 seconds) and the chamber was sealed using a valve
on the chamber. A solution of water and the chemical admixtures was introduced into the
chamber in the evacuated condition through the valve. The valve was then closed and the
chamber was placed in a commercial paint shaker at which time the system was shaken (i.e.,
mixed) for five minutes. The cement paste slurry was then placed in the molds using a
combination external vibration as described in section 3.
It should be noted that the pastes used in the corrugated tube method were initially
prepared following the vacuum method. However, the larger volume of paste required for this
test made this a cumbersome procedure and comparisons were therefore made between the
deaired mixing procedure and the ASTM C-305 [31] procedure. Virtually identical results were
obtained from the corrugated tube for mixtures prepared using both procedures and as a result
the corrugated tube was subsequently prepared using ASTM C-305 procedures.
5.0 EXPERIMENTAL RESULTS

While the previous sections have described the test methods and mixture proportions, the
following section describes the typical experimental results obtained from each of the tests.
Specifically, the following section will focus on specific test results and experimental
observations, while section 6.0 reconciles the results from the individual testing procedures and
compares it with the time of set results from the Vicat test.
5.1 Chemical Shrinkage: Specimen Thickness, Amount of Fluid, and Fluid

Composition
Figure 5a shows the influence of specimen thickness on the measured chemical
shrinkage. During the first few hours the behavior is quite similar irrespective of specimen
thickness. An initial rapid increase in chemical shrinkage occurs between 30 minutes (when the
specimen is placed in the bath) and 2 hours (Region I) that may initially be thought to be due to
the initial dissolution of the small cement particles or reaction of the tricalcium aluminate (C3A).
It should be noted, however, that Region I extends to a later time than that typically seen in
calorimetry and may also be influenced by the rapid dissolution of sulfate or temperature effects
at early ages. After an age of about 2 hours, the rate of chemical shrinkage slows down as the
cement enters the ‘dormant period’ (Region II). During the dormant period the rate of chemical
shrinkage is low (i.e., the slope of the chemical shrinkage is very flat and near zero, Figure 5c).
As the specimen approaches an age of 6 hours, the hydration reactions enter the ‘acceleration
phase’ (Region III) and the chemical shrinkage begins to increase rapidly. It can be seen that the
thicker specimen has a slightly higher rate of reaction (i.e., steeper slope) in this phase. The
faster rate of reaction may be due to a combination of a slightly higher temperature in the thick
specimen due to the exothermic reaction and the fact that the pore solution is less diluted by the
water (fluid) on the surface of the chemical shrinkage specimen.
Geiker [16] observed that increasing sample height caused a reduction in chemical
shrinkage at later ages and this was amplified in specimens with a lower water to cement ratio or
finer cement. Geiker measured differences in non-evaporable water through the specimen height
and noticed that this was less than the difference in chemical shrinkage due to the lower RH in
the specimen. The present study also showed that the chemical shrinkage in the thicker
specimens begins to plateau at an earlier age (Region IV), however a plateau appears to occur in
even smaller specimens than those observed in [16]. The authors believe that the observation of
the plateau of chemical shrinkage is presumably due to densification of the pore structure due to
hydration, which disconnects the porosity and makes it more difficult for the water to be
absorbed in a thicker specimen, as such the pores would not be filled with water. In the present
study, a 25 g and 200 g specimen were removed from the water bath and glass dish at an age of
24 hours and crushed. The crushed particles were weighed immediately after crushing (i.e., 24
hours) and immersed in water before being reweighed at an age of 48 hours. It was observed
that the 200 g specimen absorbed nearly 0.013 grams of water per gram of cement between 24
and 48 hours while the 25 g specimen only absorbed 0.007 grams of water per gram of cement
during the same time. These absorptions were both 0.003 grams less than the water absorption
that may be anticipated (Figure 5a) and it is believed that this difference exists due to the
uncertainty in measuring the water absorption on the surface of the crushed particles. This
however appears to confirm that water was limited from filling the pores in the thicker specimen
(200 g) at early ages, resulting in the chemical shrinkage voids not being completely water filled.
Chemical Shrinkage (ml/gcem)
0.04
Chemical Shrinkage (ml/gcem)

0.04
0.03 0.03
0.02 0.02
W/C = 0.30 - 25 g
W/C = 0.30 10g DI Water
0.01 25 g ( ~ 3 mm) 0.01
10g CH-P. Soln.
50 g ( ~ 6 mm) 10g P. Soln.
200 g (~ 24 mm) 40g DI Water
0.00 0.00
0 6 12 18 24 30 36 42 48 0 6 12 18 24 30 36 42 48
Age of Specimen (hours) Age of Specimen (hours)
(a) (b)
0.004
Shrinkage (ml/gcem/hr)
I II III IV V
Rate of Chemical
0.003
W/C = 0.30 - 25 g
0.002 10g DI Water
10g CH-P. Soln.
10g P. Soln.
0.001 40g DI Water
0.000
0 6 12 18 24 30 36 42 48
(c)
FIGURE 5 Measured Chemical Shrinkage: (a) Influence of Specimen Thickness, (b)

Influence of Fluid Ponded on the Specimen and (c) the Rate of Chemical Shrinkage
In addition to determining the influence of the thickness of the specimen on the measured
chemical shrinkage, Figure 5b shows the influence of the composition of the fluid that is ponded
on the chemical shrinkage specimen. To do this, a simulated pore solution (0.15 KOH + 0.05
NaOH solution, pH 13.30 or lime (CH) saturated 0.15 KOH + 0.05 NaOH solution, pH 13.27)
was prepared and ponded on the specimen in place of the deionized water (DI, pH 7.65). It can
be seen that the specimen with lime saturated pore solution shows a slight retardation as
compared with the one ponded with deionized water and the pore solution without lime shows a
slightly slower reaction. In addition to altering the composition of the ponding fluid, the amount
of the fluid was altered by adding 40 grams of deionized water (instead of 10 grams) to one
series of specimens. It can be seen that the specimen with a large volume of ponding solution
shows more chemical shrinkage initially as well as a more rapid rate of reaction. Each of these
observations is consistent with the idea that the composition of the ponding solution on the
specimen will change during the test to try to become similar to the internal pore solution. A
larger, less similar ponding solution could act to dilute the pore solution, further accelerating the
initial reactions. While further work is needed to fully understand the influence of the ponding
solution on chemical shrinkage, it is clear from these few experiments that it can alter the
magnitude of chemical shrinkage, especially if the chemical shrinkage measurements are begun
at a very early age.
5.2 Autogenous Shrinkage

Figure 6a shows the autogenous shrinkage as determined using the membrane test and the
corrugated mold method. It can be seen that for the data presented in this paper a reasonable
correlation exists between these very different test methods. This however is contrary to some of
the results reported in scientific literature where the measuring results from the volumetric
method can be three to ten times higher than the results from the linear technique [23]. This
artifact can be minimized by placing the membranes in a paraffin oil bath [24]. The data in
Figure 6a provides additional evidence for the hypothesis that, when absorption through the
membrane does not occur, a correlation can be obtained between the membrane and corrugated
tube method. In addition, it can be seen that shrinkage from the time of set in the corrugated
tube and in the membrane correspond well with linear length change measurements taken from
the horizontal length change in rigid mold and from the ASTM C-157 test (assuming a 24 hour
strain of 860 µε).
While figure 6a shows the relationship after the time of set, Figure 6b shows a
comparison of the relationship between the volumetric shrinkage that is measured using the
membrane and the shrinkage that is measured using a non-contact laser in a rigid form before set.
To do this the measured volumetric shrinkage from the membrane is assumed to initially act only
in the vertical direction. The laser measurement indicates that initially the deformation in the
rigid forms is primarily vertical settlement. This is consistent with other observations of
shrinkage at early ages [32,33,34]. The vertical displacement rate measured by the laser is
higher between 2 and 4 hours possibly due to the fact that the laser is only measuring the surface
of the paste and as such it would not account for bleed water. In addition, the effects of gravity
are more pronounced in the specimen with the rigid form. These results are consistent with the
findings of Pease et al. [27] who suggested that measurements before the time of setting should
not be considered in reporting linear shrinkage.
Linear Autogenous Strain (µε) 0 0.00
Vertical Deformation (mm)

ASTM C-157 Sealed Laser Measurement
-250 Membrane Computed from the
Corrugated Tube Membrane Test
-500 Rigid Form (Laser) 0.10
-750
-1000 0.20
-1250
-1500 0.30
0 24 48 72 96 0 3 6 9 12 15 18 21 24
Age of Specimen (hours) Age of Specimen (hours)
(a) (b)
FIGURE 6 a) Comparison of the Autogenous Shrinkage Strain Measured using the Four
Different Testing Protocols (ASTM C-157, Membrane, Corrugated Tube, and Rigid
Form)** and b) Comparison of the Vertical Deformation Measured in the Rigid Mold Using
the Laser and the Computed Vertical Deformation Assuming All the Deformation at Early
Ages Occurs in the Vertical Direction
6.0 DISCUSSION TEST RESULTS WITH THE TIME OF SET

The chemical and autogenous shrinkage results are compared to determine whether these
tests may be able to be related to material structure development. It should be noted that strictly
speaking the sealed specimens (i.e., specimens in a closed system) and specimens that are able to
absorb water from their surroundings (i.e., specimens in an open system) may not demonstrate
the same extent of hydration at the same time. Before setting this difference will be relatively
minor and only influenced by leaching, however at later ages since the supply of water from an
external source will lead to increased hydration. Figure 7 shows the chemical shrinkage as
measured using the buoyancy method, the autogenous shrinkage measured using the membrane
method, and the time of set as determined from the Vicat test. The chemical and autogenous
shrinkage are very similar initially as the fluidity of the paste does not allow creation of internal
empty pores. It can be noticed however that between 7 and 8 hours the measured shrinkage
responses begins to diverge. This is similar to the final set as determined by the Vicat test.
**
Note – Each test was zeroed at an estimated set time. The corrugated tube and rigid form methods were zeroed at 6.1 hours
which corresponds to the time of set as determined from the Vicat test. The membrane method was zeroed to the time at which it
diverged from the chemical shrinkage (Fig. 7) which corresponds to an age of approximately 7.9 hours. The ASTM C-157
Method was assumed to have a strain of 680 µε at 24 hours based on the corrugated tube measurements.
Linear Autogenous Strain (µε)

0
Vicat - Initial Set
Vicat -
-2000 Final Set
-4000
W/C = 0.30
-6000 Chemical
Autogenous
(Membrane)
-8000
0 3 6 9 12 15 18
FIGURE 7 Illustration of the Use of Chemical Shrinkage and Autogenous Shrinkage

Measurements to Determine the Time of Mechanical Property Development
7.0 SUMMARY AND CONCLUSIONS

Recently, substantial research has been performed to assess the risk of early-age cracking in
concrete used for the construction of transportation structures. Unfortunately, many existing
testing procedures for shrinkage do not always define shrinkage in a consistent manner. This is
especially critical for higher-strength, lower w/c materials, especially at early ages. This paper
reviews several shrinkage testing protocols for cementitious paste at early-ages. Results of these
test methods are compared. In summary:
• The ‘blind application’ [3] of a standard test method like ASTM C157 or C494 to the
measurement of shrinkage in low w/c materials does not provide an accurate picture of
the shrinkage that occurs in these materials. These methods do not capture the substantial
shrinkage that occurs prior to the beginning of the ASTM shrinkage test (Fig. 1). As such
the conventional standard test methods provide a false indication of early-age shrinkage.
• While several chemical shrinkage tests procedures have been used over the last century,
this paper has illustrated the benefits of a test protocol that is based on buoyancy, in that
it can be automated. This paper has confirmed that the thickness of the specimen,
thickness of the fluid layer (e.g., water in many cases) on the specimen, and chemical
composition of the fluid, all influence the initial chemical shrinkage that is measured,
however these differences are much less at later ages. This is however important for
determining when the test data should begin to be recorded and used for ‘zeroing’ the
test.
• Two primary autogenous shrinkage testing protocols (the membrane and corrugated tube)
show similar behavior at early ages, provided the membrane does not absorb water or
paraffin oil. While the membrane method is the easiest to interpret before setting since
the volumetric and linear shrinkage are easily related, the corrugated tube method is
easier to perform and repeat. When these methods are compared with measurements
performed on specimens in a rigid mold (or for specimens placed in forms in service) an
interesting observation can be made. For the specimens in the rigid form, the volume
change that occurs prior to the time of set (i.e., solid skeleton formation) occurs in the
vertical direction. This may have an important role in relating the volumetric test method
with other shrinkage test methods that are based on a linear length change. All of the test
methods show a reasonable correlation (Fig 6.) after setting.
• The divergence of measurements of chemical and autogenous shrinkage at early ages can
provide a measure of the time at which a solid skeleton forms. The divergence occurs
around the time of final set according to the Vicat test.
8.0 ACKNOWLEDGEMENTS
The authors gratefully acknowledge support phases of this research which has come from
Degussa chemical corp., the Center for Advanced Cement Based Materials and the Danish
Technical Scientific Research Council (STVF). The authors also thank Mette Geiker for her
helpful suggestions for improving this manuscript.
9.0 REFERENCES
1 Bentur, A. Early Age Cracking In Cementitious Systems, – RILEM State of the Art Report
TC-EAS, ed A. Bentur, © 2002
2 NCHRP Report 380 - Krauss, P. D., Rogalla, E. A., Sherman, M. R., McDonald, D. B.,
Osborn, A. E. N., and Pfeifer, D. W. Transverse Cracking in Newly Constructed Bridge
Decks. NCHRP Project 12-37, 1995.
3 Aitcin, P.-C., (1988) “Autogenous Shrinkage Measurement,” Autoshrink ’98, Proceedings of

the International Workshop on Autogenous Shrinkage of Concrete, Hiroshima, Japan, ed. E.
Tazawa, pp. 245-256
4 ASTM C 157 Length Change of Hardened Hydraulic-Cement Mortar and Concrete The
American Society of Testing and Materials, USA (2003)
5 La Chatelier, H., (1900) “Sur les Changements de Volume qui Accompagent le durcissement
des Ciments,” Bulletin Societe de l’Encouragement pour l’Industrie Nationale, Seme serie,
tome 5, Paris, 1900
6 Jensen, O.M. and Hansen, P.F.: Autogenous deformation and RH-change in perspective.
Cement and Concrete Research 31 (2001), pp. 1859-1865
7 ASTM C 403/C 403M, Test Method for Time of Setting of Concrete Mixtures by Penetration
Resistance, The American Society of Testing and Materials, USA (2003)
8 ASTM 191 Time of Setting of Hydraulic Cement by Vicat Needle, The American Society of
Testing and Materials, USA (2003)
9 Weiss, W. J., “Chapter 6.1 - Experimental Determination of the ‘Time-Zero’”, Early Age
Cracking In Cementitious Systems” – RILEM State of the Art Report TC-EAS, ed A. Bentur,
© 2002
10 Justnes, H., Clemmens, F., Depuydt, P., Van Gemert, D., Sellevold, E.J., (2000) Correlating
the deviation point between external and total chemical shrinkage with setting time and other
characteristics of cement pastes, Proc. Shrinkage 2000 – Int. RILEM Workshop on Shrinkage
of Concrete, Paris 2000, pp. 57-73.
11 Boivin, S., Acker, P., Rigaud, S., and Clavaud, B, (1998) “Experimental Assessment of
Chemical Shrinkage of Hydrating Cement Paste,” Autoshrink’98 Proceedings of the
International Workshop on Autogenous Shrinakge of Concrete, ed. E. Tazawa, p. 77-88
12 Hammer, T.A., (1998) “Test Methods for Linear Measurement of Autogenous Shrinkage
Before Setting,” Autoshrink’98 Proceedings of the International Workshop on Autogenous
Shrinakge of Concrete, ed. E. Tazawa, p.141-152
13 Kosmatka, S., Kerkhoff, B, and Panarese, W. C., “Design and Control of Concrete
Mixtures,” 14th Edition, © 2002
14 Powers, T. C., and Brownyard T. L., (1948) "Studies on the Physical Properties of Hardened
Portland Cement Paste" PCA Bulletin 22, Chicago, Illinois
15 Knudsen, T., and Geiker, M., ”Chemical Shrinkage as an Indicator of the Stage of
Hardening,” International Conference on Concrete of Early Ages, Volume 1, 1982, pp. 163-
165
16 Geiker, M. “Studies of Portland Cement Hydration: Measurements of Chemical Shrinkage

and a Systematic Evaluation of Hydration Curves by Means of the Dispersion Model,” Ph.D.
Thesis, Technical University of Denmark, Copenhagen, Denmark, 1983.
17 ASTM C1608, Test Method for Chemical Shrinkage of Hydraulic Cement Paste, The
American Society of Testing and Materials, USA (to be released)
18 Parrott, L.J., Geiker, M., Gutteridge, W.A., and Killoh, D., (1990) “Monitoring Portland
Cement Hydration: Comparison of Methods,” Cement and Concrete Research, Vol. 20, 919-
926
19 Rey, M., (in french) “Nouvelle metode de mesure de l’hydration des liants hydrauliques’,
Publication du Centre d’Etudes et de Recherches de l’Industrie des Liants Hydrauliques,
Revue des Materiaux, numero special octobre 1950
20 Yamazaki, Y., Monji, T., and Sugiura, K., (1976) “Early age expanding behavior of mortars
and concretes using expansive additives of CaO-CaSO4-4CaO•3Al2O3•SO3 system, Sixth
International Congress on the Chemistry of Cement, Moscow, September 1974, Stroyizdat,
Moscow III-5 (1976) 192-195
21 Buil, M., Studies of the shrinkage of hardening cement paste, (in French), (1979) D.Eng.
thesis, Rapport de recherche LPC No. 92, Laboratoire Central des Ponts et Chaussées, Paris
22 Davis, H.E., (1940) Autogenous volume changes of concrete, Proceedings of the 43rd annual
meeting, American Society for Testing Materials, Philadelphia 40 (32) 1103-1112
23 Wuerpel, C.E., (1946) Laboratory studies of concrete containing air-entraining admixtures,

Journal of the American Concrete Institute 42 (4) 305-359
24 Lura, P., and Jensen, O. M., “Measuring Techniques for Autogenous Strain of Cement
Paste,” Knud Højgaard Conference on Advanced Cement-Based Materials, Lyngby,
Denmark, June 2005 (also submitted to Materials and Structures).
25 Hammer, T.A., Bjøntegaard, Ø., and Sellevold, E.J., (2002), ‘Measurement methods for
testing of early age autogenous strain’, Early age cracking in cementitious systems, ed. A.
Bentur, RILEM TC 181-EAS Committee, RILEM, Cachan, France, pp. 234-245.
26 Jensen, O.M., Hansen, P.F., ‘A dilatometer for measuring autogenous deformation in

hardening Portland cement paste’, Mater. Struct. 28 (181) (1995) 406-409
27 Jensen, O.M., ‘Dilatometer – further development’, Building Materials Laboratory, The

Technical University of Denmark, Lyngby, Denmark, 1996, 8 pp.
28 Pease, B. J., Hossain, A. B., and Weiss, W. J., “Quantifying Volume Change, Stress
Development, and Cracking Due to Self-Desiccation,” ACI SP-220 Autogenous Deformation
of Concrete, 23-39, March 2004
29 Kim, B., and Weiss, W. J., (2003) “Using Acoustic Emission to Quantify Damage in
Restrained Fiber Reinforced Cement Mortars,” Cement and Concrete Research, Feb., 2003,
vol. 33, no. 2, pp. 207-214
30 Winslow, D.N., Cohen, M.D., Bentz, D.P., Snyder, K.A., Garboczi, E.J. (1994) "Percolation
and Pore Structure in Mortars and Concrete," Cem. and Concr. Res., 24[1] 25-37
31 ASTM C 305, Standard Practice for Mechanical Mixing of Hydraulic Cement Pastes and
Mortars of Plastic Consistency, The American Society of Testing and Materials, USA (1999)
32 Powers, T. C., “The Properties of Fresh Concrete,” John Wiley and Sons, Inc., New York, ©
1968, pp. 664
33 Kayir, H., and Weiss, W. J., (2002) "A Fundamental Look At Settlement In Fresh Systems:
Role Of Mixing Time And High Range Water Reducers," First North American Conference
on Self-Consolidating Concrete, Chicago, IL, November, 2002, pp. 27-32
34 Lura, P., Pease, B.J., Mazzotta, G., Rajabipour, F., and Weiss, W. J., “Influence of shrinkage
reducing-admixtures on the development of plastic shrinkage cracks”, Submitted to ACI
Materials Journal, 2005

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Sant, Lura, and Weiss Measurement of Volume Change in Cementitious Materials at Early Ages Page 1 of 19

Measurement of Volume Change in Cementitious Materials at Early Ages:

Jason Weiss (Corresponding Author)

Measurement of Volume Change in Cementitious Materials at Early Ages:

Gaurav Sant, Pietro Lura, and Jason Weiss

FIGURE 1 A comparison of the autogenous shrinkage measured in sealed specimens using

W/C = 0.30 Chemical Shrinkage (Bouyancy Method)

2.0 REVIEW OF TEST METHODS FOR EARLY-AGE SHRINKAGE

2.1 Chemical Shrinkage

2.2 Autogenous Shrinkage

3.0 EXPERIMENTAL PROTOCOLS USED IN THIS STUDY

3.1 Chemical Shrinkage – Buoyancy Protocol

FIGURE 3 An illustration of experimental procedures to measure chemical shrinkage: a)

∆V paste (t ) Wsub (t ) − Wsub (30 )

3.2 Autogenous Shrinkage Measurement Protocols

3.2.1 Autogenous Shrinkage – Membrane Method Protocol

Corrugated Data Conditioning

FIGURE 4 An illustration of experimental procedures to measure autogenous shrinkage:

∆V paste (t ) Wsub (t ) − Wsub (30)

3.2.2 Autogenous Shrinkage – Corrugated Tube Method Protocol

3.2.3 Autogenous Shrinkage – Rigid Form Method Protocol

3.2.4 Autogenous Shrinkage – ASTM C157 Testing Method Protocol – Sealed

3.3 Setting Time

4.0 EXPERIMENTAL PROGRAM

5.0 EXPERIMENTAL RESULTS

5.1 Chemical Shrinkage: Specimen Thickness, Amount of Fluid, and Fluid

Chemical Shrinkage (ml/gcem)

FIGURE 5 Measured Chemical Shrinkage: (a) Influence of Specimen Thickness, (b)

5.2 Autogenous Shrinkage

Linear Autogenous Strain (µε) 0 0.00

Vertical Deformation (mm)

6.0 DISCUSSION TEST RESULTS WITH THE TIME OF SET

Linear Autogenous Strain (µε)

FIGURE 7 Illustration of the Use of Chemical Shrinkage and Autogenous Shrinkage

7.0 SUMMARY AND CONCLUSIONS

3 Aitcin, P.-C., (1988) “Autogenous Shrinkage Measurement,” Autoshrink ’98, Proceedings of

16 Geiker, M. “Studies of Portland Cement Hydration: Measurements of Chemical Shrinkage

23 Wuerpel, C.E., (1946) Laboratory studies of concrete containing air-entraining admixtures,

26 Jensen, O.M., Hansen, P.F., ‘A dilatometer for measuring autogenous deformation in

27 Jensen, O.M., ‘Dilatometer – further development’, Building Materials Laboratory, The

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