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II

DETERMINATION OF THERMAL CONDUCTIVITY BY TRANSIENT

HOT WIRE METHOD
Neven Ukrainczyk1, Jurica Alekovi2, Juraj ipui1
1

Faculty of Chemical Engineering and Technology, University of Zagreb, Maruliev trg 20,
Zagreb, Croatia
2
Elektroda Zagreb d.d. Ruevje 7, 10290 Zaprei - Zagreb, Croatia

Corresponding author: N. Ukrainczyk: nukrainc@fkit.hr

Izvorni znanstveni rad / Original scientific paper

Abstract
Thermal property data are important for the engineering solutions of the heat transfer
problems. There are many cases in which thermal conductivity of the studied material is not
available, eg. cement materials of different compositions during setting and hardening.
Furthermore, these materials are wet and porous and in order to prevent development of
humidity gradients under imposed thermal gradients, one finds transient measurement
methods as preferable.
This work describes a developed apparatus and a transient Hot Wire (HW) method to obtain
the thermal conductivity of dry and wet materials. Single, thin platinum wire is used as both a
constant power heater and temperature sensor. The result obtained from measurement is the
temperature development of the HW during heating period, which is described by a
theoretical model. The thermal conductivity of the material under study is obtained by the
solution of the parameter estimation problem, utilizing the Levenberg-Marquardt method of
optimization. The results of the method evaluation on reference materials indicated an
accuracy of 3% and a uncertainty of 0.7% (for 95% confidence). The reference materials
used were gelatinous water (Agar gel 0.7%), glycerol and Ottawa (quartz) sand. The values
of the thermal conductivity for fresh calcium aluminate cement pastes with water to cement
mass ratio of 30 and 40 % are documented. The systematic error arising due to the measured
sample electrical conductivity is calculated to be less than 0.5% for the experimental
configuration used.
Keywords: thermal conductivity, hot wire method, reference materials, electrical
conductivity, calcium aluminate cement.

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1. Introduction
Material thermal property data are important for the engineering solutions of the heat
transfer problems. Measurements of thermal properties of heterogeneous, wet and porous
materials by conventional steady-state methods are subject to large errors. In order to avoid
water migration during the run-time of the thermal tests, transient measurement methods are
preferable [1, 2]. The determination of thermal conductivity is very challenging since it
belongs to a class of inverse problems where an estimated parameter is very sensitive to
measured quantities necessary for its calculation. The hot wire method [1] involves an ideal
line heat source, infinitely long with zero mass, immersed in an infinite sample. As the
parallel wire method is very sensitive to the uncertainty of measuring the radial distance of a
thermocouple from a heater, a resistance technique is employed. Furthermore, by this
method, where the wire acts as both a heater and a resistance thermometer, the influence of
local non-homogeneities of measured materials is minimized. Thermal conductivity is
determined by inverse solution of the differential equation for radial heat conduction. In
order to minimize errors due to an approximation of the used model and effects of the
experimental setup a critical design of an experimental configuration is necessary.
This work describes a developed apparatus and a method to obtain a thermal conductivity of
dry and wet materials. The systematic error due to a electrical conductivity of cement paste is
minimized by the used experimental configuration. The values of the thermal conductivity
for fresh calcium aluminate cement (CAC) pastes are documented to the best of our
knowledge for the first time and compared to the available literature data on portland cement.
Research on thermal properties of CAC is particularly interesting due to rapid heat
generation during hydration and development of significant temperature gradient in material
[3, 4].
2. Hot wire model
When a heat generation is applied to the line heat source, its temperature response is based
on an analytical solution [5] to the heat conduction model given in cylindrical coordinates:
r 2
q
t =t
(1)
E
T ( r , t )t =0 =

4
4at
where is the thermal conductivity of sample (Wm-1K-1), r is the radius of the wire (m) a is
thermal diffusivity of sample (m2s-1), t is time (s), q is rate of heat generation (W/m) and Ei is
the exponential integral computed as:
z 2 z3 z 4
Ei ( z ) = + ln z + z + + .....
(2)
2! 3! 4!

in which = 0.5772... is Eulers constant and z = r 2 /(4at ) .

3. Experiment
3.1. Materials
The reference materials used to evaluate the used apparatus and method are gelatinous
water (Agar gel 0.7%) and Ottawa sand. For detailed discussion on reference materials used
please see further in 3.3 and 4.2.

419

Furthermore, this paper documents the thermal conductivities of cement pastes obtained
with sample of commercial CAC ISTRA 40 taken from a regular production of Istra Cement
International, Pula, Croatia. The cement has the oxide mass fraction composition listed in
Table 1. Physical properties of used cement are given in Table 2. All mixes were prepared
with deionized water. The main compounds are CA (cement notation: C=CaO, A=Al2O3,
F=Fe2O3, S=SiO2, H=H2O) and ferrite phase (C4AF-C6AF2), with mayenite, C12A7, gehlenite,
C2AS and -C2S as minor compounds. Cement pastes with water to cement mass ratio of 0.3
and 0.4 were prepared.
Table 1. Chemical composition of investigated CAC.
CaO
Al2O3
Fe2O3
FeO
SiO2
TiO2 MgO
SO3
Na2O K2O
Sum
37.10% 38.47% 14.39% 2.90% 4.43% 1.05% 0.90% 0.20% 0.14% 0.17% 99.8%

>90 m,
%
3.76

Table 2. Physical properties of investigated CAC.

Bulk density, kg/m3
Blaine, Specific Setting time,
Standard
2
cm /g gravity,
min
consistency, Loose
Compacte
3
g/cm
%
d
initial final
3401
3.20
298
329
24.0
950
1776

3.2. Measuring device

The thermal conductivity is determined from the time dependant temperature rise of an
electrically heated wire. The wire used is 99.99+% platinum (Aldrich) with a diameter 2r =
76 m and length of l = 176 mm. It is desired to have a wire with as small a diameter as
possible because the theory assumes a true line heat source. The wire is heated by placing a
constant voltage across the bridge, as suggested by Glatzmaier and Ramirez [6]. The supplied
voltage has an output range of 0 25V and is stable to within 10V. Change in the wire
electrical resistance is determined by measuring the unbalanced voltage of a precision
Wheatstone bridge during heating period. This voltage is read by a computer via an 8 channel
10-bit A/D converter. Measuring apparatus is connected to the PC via RS232 protocol that
provides the sampling rate of 15ms. Specially designed programs provide control of the
automatic measuring apparatus and easy usage. The core of the measuring apparatus is a
microcontroler PIC 16F877 which was programmed in MPLab by a direct RISC instructions
and ICD-2 programmer/debugger. From the previously obtained resistance versus
temperature calibration (least-squares regression) of the used Pt wire the change of the
temperature is deduced.
The low temperature rise of hot wire, obtained by applying low input voltage, is desirable in
terms of minimizing the effects of natural convection, radiation and/or gas evolution. On the
other hand, higher voltage reduces the effect of noise and allow for a more precise
temperature measurement. In this work the applied voltage gave temperature rise of 5C
(during 2 min). Only for measurements on glycerol the temperature rise was reduced to 3C
in order to minimize the natural convection effect.

420

Figure 1. Thermal conductivity measuring setup.

3.3. Experimental setup
The mould containing the investigated sample is obtained in the following manner. The
specimens were cast in cylindrical copper containers with inner diameter 2R = 51 mm, length
250 mm and thickness of 1 mm. The Pt wire was placed in the center of the tube. A Pt wire
supported by a tensioning system is placed in the tube, the frame being next to the inside
surface of the copper pipe, Figure 1. Also the thermocouple is placed near the tube axis to
monitor the temperature of the sample. The copper tube was carefully filled with the sample
continuously applying vibrations in order to minimize air entrapment. Copper tube is sealed
with styropore and rubber stoppers and placed in the temperature controlled water bath
(0.03C).
Thermal conductivities of reference materials were determined at 20 C. Prior to loading the
Ottawa sand to mould, it was dried at 105C. The gelatinous water was prepared by mixing
0.7 % of agar powder by weight with hot (85 C) deionized water in a laboratory glass. The
mixture was heated and stirred vigorously using a magnetic stir hot plate. Once the gel was
melted, it was poured into a mold by tapping it to help the air bubbles rise to the surface. The
mold was put in a water bath at 20 C and waited for at least 4 h to attain uniform
temperature. The fresh pastes were tested at temperature 20 C during the period of 1.5 2.5
hours after mixing.
4. Results and discussion
4.1. Thermal conductivity determination
Deviations from the idealized model in Eq. (1), classified as inner and outer, can be
minimized by a proper selection of experimental conditions. Inner deviations arise from the
non-ideality of the wire that has finite length, mass and heat capacity. These deviations,
which depend on the properties of the wire, have significant impact only on the initial
temperature response (t < tmin). Outer deviations are due to the finite dimensions of the
sample and have impact at longer times (t > tmax) when the outer boundary conditions (of the
sample) influence the wire temperature response. The so-called time window defines
representative temperature response corresponding to the sample thermal properties. It is
estimated by numerical simulation supposing a systematic error of 0.1 % to be between tmin =
0.5 s and tmax = 120 s. For simulations a numerical model of one dimensional radial heat
conduction was built for the used experimental configuration and solved by using

421

MATLABs built-in solver pdepe [7, 8]. The model employed two coupled partial
differential equations of energy conservation: one for the wire and one for the sample [9].
The thermal conductivity was calculated by fitting the experimental results to a theoretical
expression (1) by using literature values for thermal diffusivity [10-12], listed in Table 3, and
eight terms for calculating the exponential integral according to the Eq. (2). This parameter
estimation problem was solved by the Levenberg-Marquardt method of optimization [13,
14]. In order to investigate the sensitivity of thermal conductivity and thermal diffusivity a
simulation analysis was performed by plotting predicted responses by Eq. (1) with 10 %
change in the investigated parameters. The results on parameter sensitivity analysis, shown in
Fig. 2, indicate a low impact of thermal diffusivity and good sensitivity of thermal
conductivity onto the temperature response (T). Therefore, an uncertainty of value on
thermal diffusivity has little impact to estimation of thermal conductivity. Data on thermal
diffusivity of fresh cement pastes are taken from independent transient measurements
conducted in our laboratory [15].
Table 3. Literature data on thermal conductivity and thermal diffusivity at T = 20 C.
Material
/ W m-1 K-1 a 107 / m2s-1
Ottawa sand
0.306 [17]
2.33 [11]
Gelatinous water (Agar)
0.5985 [10]
1.433[10]
0.962 [12]
Glycerol
0.285 [12]
Fresh cement paste w/c = 0.4
2.97 [15]
Fresh cement paste w/c = 0.3
3.30 [15]
4.5
= 0.9

4.0

= 1.0
= 1.1

T / C

3.5

a = 3.3e-7
a = 2.7e-7

3.0

a = 3.0e-7

2.5
2.0
1.5
0

20

40

60

80

100

t/s

Figure 2. Parameter sensitivity analysis. Impact of 10 % change in values of thermal

conductivity and thermal diffusivity onto the theoretical temperature response.
4.2. Evaluation on reference materials
The reference materials used to evaluate the used apparatus and method are gelatinous
water (Agar gel 0.7%) and Ottawa sand. Ottawa sand consists of spherical grains (high purity
silica) with an accurately graded particle size distribution to pass an 850- (US Standard No.

422

20) sieve and to be retained on a 600- (US Standard No. 30) sieve. Data on the thermal
conductivity of Ottawa sand in air is readily available from several sources, although no
specific standard exists for this property.
The solid density of the Ottawa sand was measured by submerging a known mass of sand in
water and measuring the volume change of the liquid. The solid density was found to be 2.69
g/cm3, which is very close to the published value of 2.65 g/cm3 [16]. Knowledge of the bulk
density is important because the thermal conductivity can change based on how tightly the
sand particles are packed. Measured bulk density of investigated Ottawa sand of 1.650 g/cm3
is close to the published value of 1.615 g/cm3 [17]. The thermal diffusivity data on Ottawa
sand were not readily found in literature. Hence, the used value in Eq. (1) is taken for sand in
general [15]. The density and thermal conductivity of investigated Ottawa sand are 2.64
g/cm3 and 0.31 Wm-1 K-1, which is close to the published value of 2.6 g/cm3 and 0.3 Wm-1K-1
[15].
Agar is gel-forming polysaccharide, widely used in industry and in scientific applications.
Agar form gels at approximately 35C and once formed does not melt below 85C. Gelation
occurs when a chain of macromolecules forms a network capable of entrapping the
dispersing medium. Such gel has a composition close to a pure liquid but resemble a solid. In
that way heat transfer through agar is by conduction solely, excluding natural convection.
A repeatability analysis was conducted on samples by repeating the measurements 10 times.
The mean values of the thermal conductivities and estimated precision at a 95 % confidence
level are listed in Table 4. Very good agreement was found between the results of the
experimental investigation and sources of available data. This finding validates the accuracy
of the measurement apparatus and provides confidence that further results are accurate. It can
be concluded that the results of the method evaluation on reference materials indicated an
accuracy of 3 % and uncertainty of 0.7 % (for 95 % confidence).
4.3. Effect of cement paste electrical conductivity
The electrical conductivity of cement paste was measured by conductivity meter (Lab 960
Schott instruments) 0.5 h after mixing cement and water. For cement pastes with water to
cement ratio 0.4 and 0.3 the measured electrical conductivities are 1287 Scm-1 and 1098
Scm-1, respectively. The resistance of the cement paste sample in a defined geometry (see
3.3) is calculated by referring to the values of the obtained electrical conductivity. The
deviation of the overall electrical resistance (of the parallel system of sample and Pt
resistance), RII from the Pt resistance is calculated to be less than 0.5 %.
Hence, in the experimental configuration the systematic error due to the electrical
conductivity of cement paste can be assumed to be less than 0.5 %.
4.4. Thermal conductivity of fresh cement pastes
Cement based material is a complex heterogeneous, multiphase and polydisperse system.
Through such a material the heat is transferred by a combination of different modes. They
include conduction through the solid particles, conduction and convection through the
gaseous and liquid phases, evaporation condensation mechanism [2], and radiation at the
particle surfaces. However, this overall process is practically modelled solely by a heat
conduction model considering the conduction parameters as apparent. Therefore, one should
bear in mind that the physical parameters measured in this paper for cement paste and Ottawa
sand are more properly called apparent thermal conductivity [2]. The values of the thermal

423

conductivity for fresh calcium aluminate cement pastes obtained show good agreement with
the literature values for Portland cement (PC) [18], Table 4.
Table 4. Measured and published data on thermal conductivity at T = 20 C.
/ W m-1 K-1
Material
Measured Uncertainty
Reported
Accuracy
Ottawa sand
0.315
0.5 %
0.306 [17]
3%
Gelatinous water (Agar)
0.615
0.7 %
0.5985 [10]
3%
Glycerol
0.290
0.6 %
0.285 [12]
2%
Fresh cement paste w/c =
0.98
0.7 %
(PC)0.97[18]
0.4
Fresh cement paste w/c =
1.06
0.6 %
(PC) 0.99 [18]
0.3

An example of a result for estimation of thermal conductivity based on the measured

temperature response (cement w/c = 0.4) and the radial heat conduction model (1) is given in
Fig. 3. A good fit with a standard deviation of 1.9 10-2 C validates the appliance of the heat
conduction model used for describing the heat transfer of investigated wet porous materials.
5
4
T / C

Data: FreshPaste w/c = 0.4

Model: hot_Tau

Chi^2/DoF = 3.6e-4
R^2
= 0.99802

P
l
a

Measured (HW)
Analytic Fit

0.9930
0.1760
3.0e-7
0.980
3.8e-5

(fix)
(fix)
(fix)
5e-3
(fix)

1
0
0

20

40

60

80

100

120

t/s

Figure 3. An example of a result for determination of thermal conductivity based on a

measured temperature response and the heat conduction model (1).
5. Conclusion
In order to minimize errors due to an approximation of the used model and effects of the
experimental setup a critical design of an experimental configuration is necessary. The
results of the method evaluation on reference materials indicated an accuracy of 3% and
uncertainty of 0.7% (for 95% confidence). The values of the thermal conductivity for fresh
calcium aluminate cement pastes with water to cement mass ratio of 30 and 40 % are 0.98 W
m-1 K-1 and 1.06 W m-1 K-1, respectively.
6. Acknowledgement

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The authors acknowledge support from the Croatian Ministry of Science, Education and
Sports under projects no. 125-1252970-2983 Development of Hydration Process Model.
7. Reference
1. Vozr L., A computer-controlled apparatus for thermal conductivity measurement by the
transient hot wire, Journal of Thermal Analysis, 46 (1996) 495-505.
2. De Vries, D. A., The Theory Of Heat And Moisture Transfer In Porous Media Revisited,
Int J Heat Mass Transfer, 30 (1987) 1343-1350.
3. Ukrainczyk, N., ipui, J., Dabi, P., Matusinovi, T., Microcalorimetric Study On
Calcium Aluminate Cement Hydration, 13. International conference on Materials,
Processes, Friction and Wear - MATRIB'08 (2008) 382-388.
4. George C.M, Industrial aluminous cements, Structure and Performance of Cements (ed.
P.Barnes), Applied Science, London, (1983) 415-470.
5. Carslaw, H.S. and Jaeger, J.C., Conduction of Heat in Solids, 2nd Ed., Oxford University
Press, London (1959).
6. Glatzmaier, G.C., Ramirez W. F., Simultaneous measurement of the thermal conductivity
and thermal diffusivity of unconsolidated materials by the transient hot wire method, Rev.
Sci. Instrum. 56 (1985) 1394-1398.
7. Skeel R. D, and Berzins M, A Method for the Spatial Discretization of Parabolic
Equations, SIAM J Sci Stat Comput, 11 (1990) 1-32.
8. Shampine L. F., and Reichelt M. W., The MATLAB ODE suite, SIAM J Sci Stat Comput,
18 (1997) 1-22.
9. Assael M. J., Karagiannidis L., Malamataris N., and Wakeham W. A., The Transient HotWire Technique: A Numerical Approach, International Journal of Thermophysics, 19
(1998) 379-389.
10. Lemmon E.W., McLinden M.O. and Friend D.G., "Thermophysical Properties of Fluid
Systems" In NIST Chemistry WebBook, NIST Standard Reference Database Number
69, Eds. P.J. Linstrom and W.G. Mallard, June 2005, National Institute of Standards and
Technology, Gaithersburg MD, 20899 (http://webbook.nist.gov).
11. Beck M. W. and Brown M. E., Modification Of The Burning Rate Of
Antimony/Potassium Permanganate Pyrotechnic Delay Compositions, Combustion And
Flame, 66 (1986) 67-75.
12. Lienhard, J.H.V, and Lienhard, J.H.IV, A Heat Transfer Textbook, 3rd ed., Cambridge,
MA: Phlogiston Press, 2006. (http://web.mit.edu/lienhard/www/ahtt.html)
13. Levenberg, K., A Method for the Solution of Certain Problems in Least Squares, Quart.
Appl. Math. 2, (1944) 164-168.
14. Marquardt, D.W., An Algorithm for Least-Squares Estimation of Nonlinear Parameters,
SIAM Journal on Applied Mathematics 11 (1963) 431441.
15. Ukrainczyk, N, Thermal Properties of Hydrating Calcium Aluminate Cement Pastes, to
be published.
16. ASTM Density OTTAWA sand C-190
17. NIST Standard Reference Database 81, Heat Transmission Properties of Insulating and
Building Materials Database, ID 1023, (http://srdata.nist.gov/insulation/)
18. Bentz, D.P., "Transient Plane Source Measurements of the Thermal Properties of
Hydrating Cement Pastes," Materials and Structures, 40 (2007), 1073-1080.

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