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Materials Today: Proceedings 4 (2017) 779–789 www.materialstoday.com/proceedings

5th International Conference of Materials Processing and Characterization (ICMPC 2016)

Characterization of Commercial Grade Paraffin wax as Latent Heat

Storage material for Solar dryers
Ashish Agarwala, R.M.Sarviyaa
,A
mechanical Engineering Department,MANIT,BHOPAL,462051,India

Abstract-

The characterization of latent heat storage material is utmost importance while designing the latent heat storage for any solar-thermal application.
The cost of commercial grade paraffin wax is lower compared to technical grade paraffin wax. Commercial grade paraffin waxes are easily
available in market and low in cost. Therefore, an experimental study is conducted in order to determine the thermophysical properties of
commercial paraffin wax produced by Indian Oil Company. The melting temperature, specific heat, latent heat is measured by differential
scanning calorimetry (DSC) analysis. Finally, the thermal conductivity has been calculated by Transient Plane Source (TPS) method with a
means of Hot Disk Thermal Constants Analyzer TPS-2500.The suitability of the investigated paraffin wax as latent heat storage material for solar
dryer was evaluated on the basis of the results of the experimental study.

©2017 Elsevier Ltd. All rights reserved.

Selection and peer-review under responsibility of Conference Committee Members of 5th International Conference of Materials Processing and
Characterization (ICMPC 2016).

Keywords:Paraffin wax; latent heat storage material; thermophysical properties,PCM.

1. Introduction

The continuous increase in demand of energy in the world and large gap between supply and demand of energy
are the main driving forces behind efforts to more effectively utilization of renewable energy sources. Solar energy
is one of the prospective sources of energy. Intermittent nature is the main drawback of the solar energy. This
drawback can be minimized to some extent by storing solar energy.

Corresponding author.
E-mail address:ashishagarwal@yahoo.com

2214-7853©2017 Elsevier Ltd. All rights reserved.

Selection and peer-review under responsibility of Conference Committee Members of 5th International Conference of Materials Processing and
Characterization (ICMPC 2016).
780 Ashish Agarwal & R.M. Sarviya / Materials Today: Proceedings 4 (2017) 779–789

Solar energy may be stored in the form of sensible and latent heat. Rock, concrete, brick are examples of sensible
heat storage materials. Latent heat storage is a more attractive form because of high energy storage capacity per unit
volume, absorbing and releasing heat at constant temperature, chemical stability, non-corrosivness, low vapour
pressure, small volume change during phase transformation etc. A large number of organic and inorganic phase
change materials (PCMs) are identified as latent heat storage material. Paraffin wax, fatty acids, salt hydrates are
examples of latent heat storage material. Thedesirable thermo-physical properties of latent heat storage materials are
(1) low supercooling (2) high density (3) small volume change during phase change (4) high thermal conductivity
(5) high latent heat of fusion [1].

Paraffin wax consists of a mixture of mostly straight chain n-alkanes CH3–(CH2)–CH3. Crystallisation of
the (CH3)-chain releases a large amount of latent heat. Latent heat of fusion and melting temperature of paraffin wax
increase with the increase of number of carbon atoms. Paraffins are available in a wide variety of melting
temperature. They are less expensive, reliable, show little volume change on melting and have a low vapour
pressure. Some undesirable properties of paraffins are low thermal conductivity, moderate flammability and non-
compatibility with plastic containers [2]. For latent heat storage, commercial grade paraffin wax is preferred due to
low in cost and easy availability in the market.
The transition temperature range of latent heat storage material should be selected such that can deliver the
energy at a suitable temperature for a given application. This is one of the important aspects for a latent heat storage
system. For majority of food product the temperature of air for drying should be in the range of 40- 60oC [2]. The
selection of a suitable phase change material (PCM) is important for designing the efficient heat storage system for
solar dryer. The characterization of phase change material is needed for selecting the suitable PCM. This requires the
measurement of thermophysical properties of the PCM [3]. Different thermal analysis methods are reported in the
literature for determining the thermophysical properties of the material. These methods are broadly classified into
two categories, namely, T-history method and Conventional calorimetry methods. Differential Thermal Analysis
(DTA) technique and Differential Scanning Calorimetry (DSC) methods are examples of conventional calorimetry
methods.

Yinpingand Yi [4] proposed the T-history method for determining the thermophysical properties of the
material. Graphs were drawn between temperature and time during the cooling of the sample against ambient
temperature,and the graphs are compared to reference material (pure water). Giavariniand and Pochetti [5]
conducted DSC analysis for measuring the thermo-physical properties of petroleum products such as paraffin waxes,
petrolatum, lubeoils, fueloils and bitumens.The latent heat, melting point were measured by DSC analysis. Flaherty
[6] also conducted DSC analysis on hydrocarbons and natural waxes for measuring different thermal properties.
They claimed that the DSC is the more useful technique for measuring the different thermal properties of petroleum
products. Different researchers [7,8] used the DSC analysis for finding the various thermo-physical property of the
materials.The thermophysical properties of the materials affecting the storage capacity and the heat transfer rate. The
thermophysical properties include a thermal conductivity, thermal diffusivity, thermal expansion coefficient, heat
capacity and latent heat. Literature review reported that the latent heat, thermal conductivity and heat capacity are
the important properties in a numerical and experimental study of PCMs [3,9]. For calculating the performance of
the system we must know the thermal properties of paraffin wax like thermal conductivity, latent heat, specific heat
etc. Therefore, Differential Scanning Calorimetry (DSC) and thermal conductivity analysis using TPS method has
been conducted in the present study, in order to determine thermophysical properties of commercial grade paraffin
wax.
 Ashish Agarwal & R.M. Sarviya / Materials Today: Proceedings 4 (2017) 779–789 781

Nomenclature

kthru through-plane thermal conductivities (W/m-K)

kin in-plane thermal conductivities (W/m-K)
ρ density (kg/m3)
Cp specific heat(kJ/kg-K)
T temperature (K oroC)
t time (h or s)
Qr power (W)
δ dirac delta function(-)
α thermal diffusivity (mm2/s)
R electrical resistance(ohm)
β temperature coefficient of resistance (oC-1)
r radius of the sensor (mm)
F(τ) dimensionless time dependent function (-)

2. Experimental setup

The experimental tests have been conducted in the laboratory in order to characterize the commercial grade
paraffin wax. Differential Scanning Calorimetry and Thermal conductivity analysis have been conducted to
determine the different thermophysical properties.

2.1 Differential scanning calorimetryanalysis (DSC)

2.1.1 Theory of the DSC analysis - DSC is a technique to determine the thermal behavior of material at different
temperature. It is a useful tool for thermal analysis. In this technique the reference and sample are heated such that
the temperature of the both is maintained at nearly same level. In this method the difference of heat required to
increase the temperature of reference and sample at the same level is measured. The differential heat flow is plotted
against temperature, the resulting curve is used to determine the phase change transitions, melting point,
crystallization temperature, and thermophysical properties. In the present study Differential scanning calorimetry
(DSC) analysis has been conducted to measure the melting temperature, latent heat and specific heat of the paraffin
wax.
During the test inert gas, usually nitrogen gas flow in to sample pan to maintain the inert atmosphere,
which is necessary to reduce the risk of condensation inside the DSC instrument when the temperature gets below
the air dew point and to remove corrosive gases generated from the sample during the test. The cooling/ heating
temperature rates are usually in the range of 5 - 40°C/min. If the sample is heated or cooled above the 40 °C/min,
effects of non-linearity become dominant and the calibration parameters become no longer applicable [10]. Close
thermal event can be observed at lower temperature rates, but the weak phase change event can be observed at
higher temperature rates.
782 Ashish Agarwal & R.M. Sarviya / Materials Today: Proceedings 4 (2017) 779–789

2.1.2 Apparatus and test procedure

Fig. 1 Differential scanning calorimeter used in the study. [11]

In the present study DSC analysis was performed on a Thermal Analyzer DSC 6000, TA instrument in
heating and cooling cycle (Fig. 1). The specifications of the instrument are listed in Table 1. The instrument was
calibrated using Indium standard. At the beginning of experiments the 10 mg of solid sample sealed in hermetic
pans were taken for the analysis. The sample was weighed in an analytical weighing balance. Reference and sample
aluminum pans are placed in DSC. The empty pan was used as reference. The analyses were performed in the
temperature range of -10.00°C to 170.00°C with a heating and cooling rate of 10.00°C/min and under a constant
stream of nitrogen at a constant volume flow rate.

Table 1 Specifications of Differential scanning calorimetry (DSC 6000)

Specification Value
Temperature range -180 to 450oC
Temperature accuracy ±0.1oC
Temperature precision ±0.02 oC
Sensitivity 0.02 μW
Principle Heat flux type
Heating/cooling rate 0.1 to 100oC/min

2.2 Transient Plane Source (TPS) method for measurement of Thermal Conductivity

2.2.1 Theory of the TPS Method

In the present study the Transient Plane Source (TPS) method is used for measurement of thermal conductivity of
the paraffin wax sample. Transient plane source method, sometimes also called the Hot Disk Method, is useful for
the measurement of thermal conductivity, thermal diffusivity [12]. The TPS sensor consists of a resistive element in
the shape of double spiral and this sensor act as a heat source and a resistance thermometer, for recording the
transient increase in temperature.
The TPS sensor is sandwiched between two identical halves of specimen. A constant electric current passed through
the sensor for a short duration of time. The generated heat in the sensor flows into the two halves of the samples,
through the insulation layer. The temperature of the sample and sensor increases with time. The rate of this
temperature rise depends on the thermal conductivity of surrounding material. If the thermal conductivity of the
surrounding material is low, then the rate of temperature rise of the spiral is high. The mathematical equation used in
 Ashish Agarwal & R.M. Sarviya / Materials Today: Proceedings 4 (2017) 779–789 783

the TPS method is suggested by Gustafsson [12].The heat conduction equation for a double spiral shaped element
can be approximated by considering a series of concentric equally spaced ring sources [13,14,15,16] and is given as
follows.
2
(ρC p ) ∂T = kin 1  ∂  r ∂T   + kthru ∂ T2 + ∑ Qrδ (r − r ' )δ ( z) (1)
∂t r  ∂r  ∂r   ∂z rings

where kthru and kin are the through-plane and in-plane thermal conductivities of the sample. ρ, Cp, T are the density,
specific heat and temperature of the sample respectively.t is the time of the measurement, Qr is the power supplied
to double spiral shaped element per unit length, δ is the Dirac delta function. The power supplied to each concentric
ring is proportional to the circumference of the ring. The different terms in the equations were represents the heat
accumulation, radial heat equation, axial heat conduction and heat source so that the neat heat balance equation is
established.In the transient plane source technique the sample is assumed as an infinite domain. This condition can
be applied if the experimental time is less than the characteristic thermal diffusion time. The experimental time must
be satisfied the following two conditions:
t << (D / 2 ) / (α in )
2
t << x / (α thru )
2
and (2)

where α is the thermal diffusivity of the material.

The transient temperature increase of the sensor depends on the change in electrical resistance of the sensor material
and is measured by following equations [15,16].
1R 
∆T =  n − 1
β  Rno 
(3)
where Rno and Rn is the electrical resistance of the sensor material at time 0 and t, β is the temperature coefficient
of resistance of the material, ΔT is the increase in temperature at time t. The transient temperature increase is
further correlated with the in-plane and through-plane thermal conductivities as used in equation (1) and defined as
follows [13,14].
P
∆T = F (τ )
π 3/ 2
R k in k thru
(4)
where P is the input heating power to the sensor, t is the transient measurement time, R is the radius of the sensor,
and F(τ) is a dimensionless time dependent function of α, t and R and defined as follows

τ = α int / R 2
(5)
By measuring the variation of temperature of the sensor with time, it is possible to solve the partial differential
equation of heat transfer by using iterative methods and the thermal properties such as thermal conductivity and
specific heat of the material can be calculated.

2.2.2 Apparatus and test procedure

In the present study, thermal conductivity measurements are conducted using Transient Plane Source (TPS) method
with a means of Hot Disk Thermal Constants Analyzer TPS-2500. The specifications of the instrument are listed in
Table 2. This system can measure thermal conductivity in the range of 0.005 to 1800 W/m K with an accuracy of
5%. The sensor used in this method is in the form of a circular double spiral. The 10µm thick nickel foil, in the form
of circular double spiral, sandwiched between two 25.4 µm thick layers of kapton (polyimide film). The radius of
nickel foil is 3.189 mm. Kapton film provides mechanical strength to the foil and electrical insulation to the sensors.
Fig.2 shows the Hot Disk Thermal Constants Analyzer used in this study. This apparatus consists of a sample holder
and the main processing unit (Fig. 3).
784 Ashish Agarwal & R.M. Sarviya / Materials Today: Proceedings 4 (2017) 779–789

Fig. 2 Hot Disk Thermal Constants Analyzer

Fig. 3 The detailed side and top view of the sample holder and sensor.

Two identical circular shape halves of the samples are prepared and the double spiral sensor is sandwiched between
them. The diameter and thickness of two identical circular shape halves of the samples were 6.4 cm and 3.2 mm
respectively. Two halves of the samples are sandwiched between the sensor as shown in Fig. 4 to ensure that heat is
not penetrating completely in the axial direction and to fulfill assumption of an infinite sample domain.
 Ashish Agarwal & R.M. Sarviya / Materials Today: Proceedings 4 (2017) 779–789 785

Fig. 4 Position of sensor in TPS method

After some initial testing it was decided to perform all measurements with a heating power of 4 mW with a
measurement time of 2 seconds. These two parameters were chosen to produce a large enough range of viable data
points and a large enough temperature gradient to ensure the accuracy of the measurement. At the start of the
measurement the wheatstone bridge is balanced and a drift measurement is performed. The sensor is then heated
with the selected power for the selected time and the temperature increase is recorded in 200 data points. Once the
transient recording is completed a drift graph and a transient graph are displayed. The thermal conductivity of the
sample is determined by temperature rise as a function of time using the equation (4).

Table 2 Specifications of Thermal Constants Analyzer TPS-2500

Specification Value
Thermal Conductivity 0.005 to 1800 W/m-K.
Thermal Diffusivity 0.1 to 1200 mm²/s.
Specific Heat Capacity Up to 5 MJ/m³K.
Measurement Time 1 to 1280 seconds.
Reproducibility Typically better than 1 %.
Accuracy Better than 5 %.
Temperature Range -253 °C to 1000 °C.
Thermal Conductivity 0.005 to 1800 W/m-K.

3 Result and discussion

3.1 Results of DSC analysis

The DSC curve of the paraffin wax sample is shown in Fig 5. The sharp peak (main peak) represents solid-liquid or
liquid-solid transformation during melting and solidification respectively, and the minor peak to the left of the main
peak represent solid-solid transformation [17]. The melting point of the paraffin wax is calculated by reading the
temperature at which the tangent to the maximum rising slope of a DSC curve during melting intercept the base line.
786 Ashish Agarwal & R.M. Sarviya / Materials Today: Proceedings 4 (2017) 779–789

This is called as onset point or transition temperature [18]. The area under the main and minor peak of the curve
represents the latent heat of fusion. The latent heat of fusion is calculated by numerical integration of the peak area
of the main and minor peak of thermal transition. The transient variation of specific heat of paraffin wax is shown in
Fig. 6. The measured thermo-physical properties of paraffin wax are listed in Table 3.

Fig 5. DSC curve of paraffin wax sample

Table 3. Thermo-physical properties of paraffin wax

Property Value

Melting temperature range (oC) 41 - 55

Latent heat capacity (kJ/kg) 176

Specific heat (kJ/kg-K) 2.8

*Black line - Specific heat, Red line – Heat flow

Fig.6 Specific heat curve by DSC analysis of PCM
 Ashish Agarwal & R.M. Sarviya / Materials Today: Proceedings 4 (2017) 779–789 787

3.2 Results of thermal conductivity measurement by TPS method

The drift and transient curve of the paraffin wax sample by TPS method is shown in Fig. 7 and Fig.8 respectively.

0.020

0.010
Temperature drift

0.000
0.00 5.00 10.00 15.00 20.00 25.00
-0.010

-0.020

-0.030

-0.040

-0.050

-0.060
Time (sec)

Fig.7Drift graph (Temperature vs Time)

The drift graph shows good stability as shown in Fig 7. The temperature in the drift graph is recorded for 20 sec just
before the transient measurement. From the drift graph it was found that the data points are uniformly distributed in
the graph which shows the isothermal heating of the sample. For accurate measurement data points should be
uniformly scattered in the graph, which shows the isothermal conditions for the sample which is a necessary
condition for obtaining transient chart [19,20]. Drift graph shows upward and downward trends if the sample is not
uniformly heated.

16
14
Temperature Increase (K)

12
10
8
6
4
2
0
0 50 100 150 200 250 300 350
Time (sec)
Fig.8 Transient curve of the sample
Transient curve shows the increase of the sensor temperature during heating of the sample. The rapid rise in the
temperature shows in the initial stage of heating and temperature rise progressively reduces with time. The rapid rise
in the initial stage is due to contact resistance between the sensor and the sample. The rate of rapid rise depends on
the thermal properties of the sample and varies from sample to sample. This part of the transient curve is not
788 Ashish Agarwal & R.M. Sarviya / Materials Today: Proceedings 4 (2017) 779–789

included for measurement of thermal conductivity. The thermal conductivity of the sample is determined by
temperature rise as a function of time using the equation4. The measured thermal conductivity of the paraffin wax
sample was 0.21 W/m-K.

3.3 Comparison of results with literature

The measured thermal properties of paraffin wax are agreed well with the available literature values [21-23] as
shown in table 4.The comparison of calculated and the available literature value of thermal conductivity of paraffin
wax shows that the TPS method is a reliable method for the determination of specific heat. Table 4 shows a
comparison of measurements made on a specimen of paraffin wax with the values found in the literature.

Table 4. Comparison of measured thermal properties with values found in the literature

Thermal
Melting temperature Latent heat Specific heat (liquid) Specific heat (solid)
conductivity
(oC) (kJ/kg) (kJ/kg-K) (kJ/kg-K)
(W/m-k)
Present study 55 176 2.9 2.7 0.21
Ettouney et al. [21] 52 210 2.1 2.9 0.24 (solid)
Regin et al. [23] 59.9 190 2.0 2.15 0.24 (solid)
Alkilani et al. [22] 53 189 - 2.5 0.2

4.Conclusion

An experimental study has been conducted in order to determine the thermal properties of commercial paraffin wax
produced by Indian oil company,and to evaluate their potential use as a latent heat storage material. Thermal
analysis of paraffin wax by DSC analysis shows the solid-solid transitions prior to melting and a large melting range
during melting. The sample of paraffin wax melts in the temperature range between 41 to 55oC and measured latent
heat of fusion was 176 kJ/kg. The measured thermal conductivity of the paraffin wax sample was 0.21W/m-K by the
transient plane source method. Measured thermal properties of the paraffin wax in this study are in good agreement
with the values found in the literature. Based on laboratory tests, commercial paraffin wax is found to be promising
PCM for solar dryer applications. The investigated paraffin wax possesses satisfactory thermal properties to be used
as latent heat storage material for solar dryer application in spite of its low thermal conductivity. The thermal
conductivity enhancement methods such as high thermal conductivity fins or additives should be used or formation
of composite with a material of high thermal conductivity should be prepared for high heat transfer during melting
and solidification.

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