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Construction and Building Materials 18 (2004) 145–154

Continuous monitoring of setting and hardening of mortar and concrete


H.W. Reinhardt, C.U. Grosse*
Institute of Construction Materials, University of Stuttgart, Stuttgart, Germany

Received 15 September 2003; received in revised form 12 October 2003; accepted 12 October 2003

Abstract

Two main properties of cementitious mortar and concrete are most important, i.e. rheology and setting and hardening. Rheology
determines workability and compaction ability. Setting determines the end of workability and hardening is responsible for strength
gain and stiffness development. Rheology and setting are measured in practice by rather conventional methods, which do not lead
to a continuous monitoring of properties as a function of age. A testing device was developed which utilizes the velocity of
ultrasound (US)-waves in order to continuously monitor the setting and hardening of cementitious materials. Two development
steps are emphasised, i.e. the design of the container and the exact determination of the transmitted US-pulse. It was shown that
the method leads to very reproducible results. While the beginning of setting can be determined from the velocity vs. age of
mortar curve by a mathematical procedure, the final setting is still due to empirical experience. The method is adjusted to concrete
and can also be used for other materials like gypsum, lime, starch and other stiffening materials. It can be used for quality control
in production of admixtures and new binders and for control of constancy of concrete production.
䊚 2003 Elsevier Ltd. All rights reserved.

Keywords: Mortar; Concrete; Setting; Hardening; Monitoring; Ultrasonic

1. Introduction 2. Wave propagation methods

2.1. Reflexion method


RILEM as the worldwide operating organization for
research and testing of building and construction mate- The reflexion method uses a pulse which is reflected
rials and structures has set up a Technical Committee at the boundary of a known material and the material
on ‘Advanced testing of cement based materials during to be investigated. If a pulse travels through a medium
setting and hardening’ (TC 185-ATC) which deals with and encounters a boundary with different acoustic impe-
methods detecting changes in the electrical and physical dance it is partly reflected and partly transmitted.
properties of early age concrete. The committee is Assume Z1 is the impedance of the material with the
preparing a state-of-the-art report on electrical methods, incident wave and Z2 is the impedance of the connected
nuclear magnetic resonance, wave propagation, the material then the reflexion ratio is given by
maturity method and acoustic emission. The purpose of
this paper is not to describe all those methods since Ar Z1yZ2
rs s (1)
other contributions in this volume will deal with some Ai Z1qZ2
of them, but rather to focus on the wave propagation
methods. In the following, the reflexion method is with Ar, amplitude of reflected wave and Ai, amplitude
explained and the transmission method is tackled in of incident wave. The impedance is
more detail.
ZsEyv (2)
*Corresponding author. Tel.: q49-711-685-3323; fax: q49-711-
685-7681. with E, Young’s modulus and v, stress wave velocity in
E-mail address: grasse@iwb.uni-stuttgart.de (C.U. Grosse). the respective medium. In the 1D case if the cross-

0950-0618/04/$ - see front matter 䊚 2003 Elsevier Ltd. All rights reserved.
doi:10.1016/j.conbuildmat.2003.10.002
146 H.W. Reinhardt, C.U. Grosse / Construction and Building Materials 18 (2004) 145–154

Fig. 1. Principle of transmission method.

section remains the same Zs(Er)1y2 with r, density of instance by an impactor, and recorded at both sides by
the material. a receiver, or the pulse can be imposed by an ultrasound
¨ ¨ et al. w1x have designed a steel mold to which
Ozturk (US) transmitter. In both cases the incident pulse and
two sensors are mounted, one for longitudinal waves the transmitted pulse are recorded, converted to a digital
and the other for shear waves. At the bottom of the signal and stored in a memory.
mold the waves are reflected. With increasing stiffness
of the mortar which is filled into the mold the reflexion 3.2. Container
coefficient decreases. Valic w2x has used a device with
a wave-guide which transmits the incident pulse to a There are several requirements on the container:
sample holder. Principally speaking it is a similar device ● the compressive pulse has to be transmitted through
which allows to measure the reflected wave. For more the mortar as directly as possible
details it is referred to the original Ref. w2x. The ● there should be no transmission through the container
advantage of the reflexion method is that only the walls
amplitude of the reflected pulse has to be measured and ● the transducers have to be coupled as reliably as
access is only needed to one side of the material. possible
● the filling, handling, mounting and demounting pro-
2.2. Transmission method cedures should be as easy as possible
● the procedure should allow to receive repeatable and
In the transmission method, a container is filled with reproducible results
mortar or concrete and a pulse is generated and sent ● the container should be suitable for multiple use, and
through the material. When the pulse travels from the finally,
front side of the container to the rear side during time ● waste material should be minimized.
Dt, the velocity is given by
Fig. 2 shows the results of the development of the
container. It consists of two polymethacrylate (PMMA)
vsdyDt (3) walls which are tied together by four screws with spacers
(Fig. 2a).
with d, width of the container. In this case, it is The mold is a U-shaped rubber foam element. The
extremely important to measure the travel time Dt very rubber foam has a high damping that suppresses waves
accurately. In the following, two aspects addressed, i.e. from travelling through the mold. The PMMA side walls
the development of a testing device for the transmission are large enough and disconnected such that a pulse
method and the automated measurement of the travel cannot travel around the mortar. Looking to Fig. 2b one
time. can see that the US-transmitter and receiver are inserted
in the walls such that only a small position of the wall
3. Wave transmission measuring device material remains between transducers and mortar.
The handling procedure is very easy. Mounting and
3.1. Principle demounting can be performed in a minute. After the
test, the PMMA can be cleaned with water and the mold
The principle of the transmission method is shown in could be cleaned, or more reliably, discarded and
Fig. 1. A pulse is generated at one surface of the replaced by a new one. The mold is very inexpensive.
specimen and the onset of the pulse is picked at the The volume of the mold is approximately 45 cm3, which
other side. The pulse can be generated mechanically, for is minimal. It turned out that the container fulfilled all
H.W. Reinhardt, C.U. Grosse / Construction and Building Materials 18 (2004) 145–154 147

Fig. 2. Isometric view (a) and views (b) of the container w8x.

requirements after many test series. Fig. 3 shows a close The equipment is triggered automatically on intervals
view of the container. which are chosen by the operator in advance. Depending
on the binder, the intervals are 5–10 min. Once the
3.3. Hardware container is filled with mortar and compacted, the
transducers are connected to the hardware as shown in
The schematic of the US-measurement consists of
Fig. 4 so that the first measurement can be taken several
various elements which are depicted in Fig. 4. The
minutes after mixing of the mortar. All subsequent
frequency generator is connected to the amplifier that
measurements are taken and stored automatically.
generates a signal for the US-transmitter. Both transduc-
ers, i.e. transmitter and receiver, are broad-band conical
3.4. Software
transducers sensitive in a frequency range of 20–300
kHz. The frequency has to be low because mortar is a
Using US-methods the degree of hardening is char-
highly damping material, which does not allow to use
acterized by the change of several parameters. Not only
high frequencies. The transmitted analogue signal is
the travel time of the ultrasonic pulse through the testing
digitized in an AyD converter that is a transient recorder
device, consequently the velocity of compressional
with 12 Bit amplitude resolution and 10 MHz sampling
waves are recorded but also the frequency content and
rate per channel.
the relative energy are recorded.
The file-size of a single US-measurement, e.g. one
The software developed at the University of Stuttgart
signal, contains between 32 and 300 KB. Three thousand
called FRESHCON2 is able to do an online data analysis
signals use in average not more than 1 GB on a hard
during the experiment in such a way that the operator
disc. The data are transferred via intranet of the labora-
has still some control about the tests. A screen-shot
tory to the workstation or PC of the operator. The results
showing the software at the end of an experiment is
are made visible on a monitor.
shown in Fig. 5. Continuously the US-signals with their
Fourier transform (using an FFT algorithm) are recorded
and plotted in the window at the upper left and lower
left, respectively. The shown graphs are representing the
last transmitted signal and its frequency content—the

Fig. 3. Close view of the container. Fig. 4. Schematic of US-measurement.


148 H.W. Reinhardt, C.U. Grosse / Construction and Building Materials 18 (2004) 145–154

Fig. 5. Snapshot of the screen shown by the FRESHCON2-software after the US-measurements at a reference mix.

whole experiment was finished after 22 h. As a recording 4.1. Hinkley criterion


interval 10 min was chosen. In the upper right window
the compressional wave velocity as well as the energy A signal is evaluated with respect to its energy
are plotted, calculated continuously using the onset time content. However, the energy content of the noise of the
of the signal and the signal amplitudes, respectively. signal may blur the results and it is not easy to
Both parameters are changing significantly during the distinguish between noise and real meaningful signal.
hardening of the material. Using the offline version of Therefore, a certain value is subtracted from the energy
the FRESHCON picking algorithm, the data can be re- and only if the subtraction reaches a certain value the
evaluated after the test concerning the onset times of procedure is stopped. Eq. (4) shows the energy of data
the signals only. Surprisingly, curves re-picked by the
operator are usually very similar to the automatically
processed data so that a time consuming manually
picking is not improving the results anymore.
Further on as a new feature of the FRESHCON system
the ability to record the temperature evolution over the
time is introduced as well as the determination of the
associated hydration heat, following DIN-EN 196 part
9 and Ye et al. w7x.

4. Rational determination of transmission time

In the beginning of the research the data were evalu-


ated by hand, i.e. the time signal was displayed on the
PC screen and the onset time was determined from the
first peak which occurred in the signal. This procedure
was very time consuming and many times inaccurate
when the noise of the signal was large. So, it was
decided to look for a better evaluation method which
was found in the Hinkley criterion and in the wavelet
transform. Fig. 6. Energy of the signal and Hinkley criterion.
H.W. Reinhardt, C.U. Grosse / Construction and Building Materials 18 (2004) 145–154 149

Fig. 7. Signal and Hinkley criterion with adjusted value of a.

Fig. 8. Recorded signal (above) and evaluated picking time (below).

Fig. 9. Wavelet function (a) Mexican hat, (b) Morlet.


150 H.W. Reinhardt, C.U. Grosse / Construction and Building Materials 18 (2004) 145–154

Fig. 10. Sine waves with Fourier transform (a) and wavelet transformation (b).

points 0-k-i a certain value and which is decreased by Smin until the
threshold value l is reached. Then it is stated that the
i energy increase is due to real signal whereas the previous
Sis 8 xk2 (4) energy is attributed to the noise. The time step n
ks0
indicates the onset of the arrival time. To apply the
Hinkley criterion a negative trend is subtracted
where Si is the partial energy and xk is the kth signal
sample of signal x. S9jsSjyiSny(aN) (6)
The Hinkley criterion w3x states
where Si9 is the new statistic of x, a is the trend
Snymin Sk)l for 1-k-n (5) parameter and N is the signal length in samples.
It turned out that a is usually chosen between 5 and
Looking to Fig. 6 one can see the energy which has 20. A small a leads to a too late picking time whereas
H.W. Reinhardt, C.U. Grosse / Construction and Building Materials 18 (2004) 145–154 151

Fig. 11. Original signal (above) and denoised signal (below) w5x.

a small a may lead to a too early picking time. Fig. 7 This procedure can even be improved if wavelet
illustrates the situation. In the example the best evalua- techniques in combination with a digital band-pass filter
tion would occur for as5. are used to enhance the signal-to-noise ratio w10x.
To illustrate the quality of the evaluation procedure Software can be designed to work automatically with
Fig. 8 shows above a recorded signal and below the large data sets of up to several thousand US-signals
first 200 time steps enlarged with indication of the acting as a pre-processor followed by picking algorithms
picking time. This procedure has been implemented in and an automatic onset time determination for reliable
the software FRESHCON w5x and can be used in an velocity measurements. Band-pass filtering alone is inef-
automated way. fective since signal energy is partly in the noise band.
Usually, the raw data are transformed to the wavelet
4.2. Wavelet transformation domain, where a threshold is automatically determined
separating signal from noise w5x. A discrete or a contin-
The wavelet transformation is a mathematical proce- uous wavelet transform is applied and after cutting off
dure for the evaluation of signals w4x. Opposite to the the noise the signal is transformed back to time domain
well-known Fourier transform the wavelet-transformed using an inverse wavelet transform. Additionally, a band-
signal shows the frequency domain and the time domain. pass filter can be applied as well as different mother
The wavelet transformation is shown in Eq. (7) wavelets (Fig. 8).
Fig. 11 is an example of a denoised signal. The upper
q`
signal is the original one with much noise and a low
f(a, b)s1yya | f(t)cw(tyb)yaxdt
y`
(7)
superimposed signal. If the wavelet transform together
with the frequency is applied, the lower signal shows
with f(t)ssignal, c(t)swavelet function, asscale var- clearly the onset time of the real signal. This procedure
iable and bsshift parameter w6x. There are numerous has now been programmed in a separate software code
wavelet functions, called mother wavelet, in the litera- and allows an even better evaluation of signals in
ture and only two of them are shown in Fig. 9. These combination with the Hinkley criterion.
are widely used in technical applications.
A simple application is shown in Fig. 10 with a
5. Specimen preparation
regular sine wave of four frequencies in different order.
The application of a fast Fourier transform (FFT) to
both signals leads to the picture in Fig. 10a which shows For the investigations on mortar, samples of
four distinct resonance frequencies but the time domain cement:water:fine sand according to CEN 196 in the
is lost. One cannot state from the figure which frequency proportion of 1.0:0.5:3.0 were mixed. The sand has a
appears first and which one last. Fig. 10b is the wavelet continuous grading between 80 mm and 1.6 mm. The
transformed signal which shows on the vertical axis a container of the monitoring device is filled during
relative value of the frequencies and on the horizontal vibration on a vibrating table during 2 min. Then, the
axis the time when these frequencies occur. transducers are connected to the recording equipment
152 H.W. Reinhardt, C.U. Grosse / Construction and Building Materials 18 (2004) 145–154

Fig. 12. Wave propagation velocity vs. age of the mortar with CEM Fig. 13. Wave propagation velocity vs. age of the mortar with CEM
42.5 N. 52.5 N.

and the measurements can start after about several method is when the production of admixtures should be
minutes after mixing. continuously checked.
Since shrinkage of the mortar could lead to a decou-
pling of the mortar and the container walls a layer of 6.2. Reproducibility
water is put on top of the mortar which fills the gap
when indeed a small gap would develop. Finally, the Three mortar mixes with the same composition were
whole arrangement is covered by a plastic sheet. manufactured and tested with the same equipment. Fig.
15 shows the results. The measured velocities vary only
6. Test results and discussion approximately 1%. This means that the material scatter
is very small and the equipment’s reproducibility is very
high.
6.1. Wave propagation velocity
6.3. Initial and final set
Meanwhile, numerous test series have been carried
out and three of them is shown. Fig. 12 shows results For the practical application of the results it is rather
with a Portland cement CEM I 42.5 N which is a important to know when the material starts setting and
medium rapid hardening cement according to EN 197- finishes setting. After beginning of set one cannot mix
1. The velocity of a longitudinal wave is given on the anymore and after end of setting the mix is not workable
vertical axis while the horizontal axis shows the age. anymore. It turned out that the point of first maximum
Starting with a value approximately 600 mys the veloc- in curvature of the velocity vs. age plot is the initiation
ity increases steeply at approximately 2 h. It increases
continuously until 3500 mys. Three water–cement ratios
have been tested: 0.50 (which is standard in EN 196-
1), 0.55 and 0.60. The differences are rather small.
Fig. 13 shows the results of mortar with a rapid
hardening Portland cement CEM I 52.5 N. The velocity
in mortar of fresh state started again at approximately
600 mys and increased then to 4200 mys for a water–
cement ratio of 0.50, to 4000 mys for wycs0.55 and
to 3400 mys for wycs0.60. Rapid hardening cement is
sensitive to the water–cement ratio as the velocity is
concerned.
A third series is shown in Fig. 14. Various admixtures
have been used: an accelerator, an air entraining agent
and a retarder.
The effect of the retarder is most clear whereas the
others are less prominent. All other properties were kept Fig. 14. Wave propagation velocity vs. age of the mortar with CEM
constant. This last picture shows how effective the 42.5 N and various admixtures.
H.W. Reinhardt, C.U. Grosse / Construction and Building Materials 18 (2004) 145–154 153

Fig. 15. Results of three tests with same composition.

Fig. 16. Illustration of beginning and end of setting.

of setting. This point can be determined precisely and method leads to very reproducible results. While the
mathematically. The end of setting is still under discus- beginning of setting can be determined from the velocity
sion but practical experience showed that the velocity vs. age of mortar curve by a mathematical procedure,
of 1500 mys could define it. Fig. 16 illustrates the the final setting is still due to empirical experience.
situation for a mortar with CEM 42.5 N and a wycs More information is available in Ref. w9x.
0.60. The method is adjusted to concrete and can also be
used for other materials like gypsum, lime, starch and
7. Conclusion and outlook other stiffening materials. It can be used for quality
control in production of admixtures and new binders
A testing device has been developed which utilizes and for control of constancy of concrete production.
the velocity of US-waves in order to continuously
monitor the setting and hardening of cementitious mate- Acknowledgments
rials. Two development steps are emphasised, i.e. the
design of the container and the exact determination of The contributions of the co-workers Mr Ruck (Dipl.-
the transmitted US-pulse. It has been shown that the Phys.), Mr Bahr and Mr Schmidt are gratefully acknowl-
154 H.W. Reinhardt, C.U. Grosse / Construction and Building Materials 18 (2004) 145–154

edged. Part of the work has been supported by DFG control of concrete. In: Reinhardt HW, editor. Testing during
(German Research Council) in the cooperative project concrete construction.Chapman and Hall, 1991. p. 122 –37.
w7 x Ye G, van Breugel K, Fraaij ALA. Experimental study and
SFB 381.
numerical simulation on the formation of microstructure in
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USWR Method, apparatus and application examples. Cement 259.4 at German Patent Office, Munich, 1999. European and
Concrete Res 2000;30:1633 –40. US American registration no. 09y857,536, 2001.
w3x Grosse CU, Reinhardt HW. Schallemissionsquellen automatisch
w9 x Grosse CU. About the improvement of US measurement
lokalisieren. Mater Test 1999;41(9):342 –7.
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w4x Kaiser G. A friendly guide to wavelets.Birkhauser, 1994. p.
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w5x Grosse, CU, Motz, M, Reinhardt, HW, Kroplin, ¨ H. Signal w10x Grosse C, Ruck H-J, Bahr G. Analyse von Schallemissionssig-
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