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Article history: The thermal properties including the thermal conductivity (l), the specific heat (cp), the melting and
Received 18 September 2014 crystallization temperatures together with their corresponding transition heat enthalpies of the odd-
Received in revised form numbered linear alkane hydrocarbons n-pentadecane, n-heptadecane and n-nonadecane were
19 February 2015
measured in both the solid and liquid phases using the transient hot wire and the differential scanning
Accepted 2 March 2015
calorimetry (DSC) techniques. The obtained results were compared with available literature data. Dis-
Available online 31 March 2015
cussions were based also on the X-ray diffraction spectra of the three n-alkanes carried out at different
temperatures and including both solid and liquid phases. A discontinuity of l is observed at the solid -
Keywords:
Solid/liquid phase change
liquid phase transition of the three n-alkane hydrocarbons.
Alkane hydrocarbons © 2015 Elsevier Masson SAS. All rights reserved.
Thermal conductivity
Specific heat
Melting temperature
Melting enthalpy
http://dx.doi.org/10.1016/j.ijthermalsci.2015.03.001
1290-0729/© 2015 Elsevier Masson SAS. All rights reserved.
140 C. Velez et al. / International Journal of Thermal Sciences 94 (2015) 139e146
et al. [7] we shall refer here to the lower temperature solid phase as vacuum, then cooled at 1 K/min up to 261 K. Subsequently, while
‘Ordered Solid (OS)’, while the intermediate solid phase shall be the temperature of the holder increased at 0.5 K/min, XRD dif-
referred to as ‘Disordered Solid (DS)’. The corresponding two phase fractograms were obtained every 2 K until the sample melting
transitions are ‘od’ for ordered solid to disordered solid, and temperature was reached. Data was normalized with the XPert
melting (m) for disordered solid to liquid. For the three alkanes HighScore software (Panalytical), after which the position and
investigated here, the transition temperatures Tod and Tm are shape of the different peaks were obtained by fitting to pseudo-
relatively close [5,7], leading to a complex melting behavior, that Voigt functions. Finally, from the peak positions, the structure
might provide a well-defined model system for studying the was analyzed and the corresponding constants were obtained with
sometimes complicated crystallization of polymers, surfactants, the help of the Fullprof Suite software.
lipids, etc [14,15]. The thermal conductivity (l) was measured with a versatile
For l measurements, the transient hot-wire technique was used. custom transient hot-wire calorimeter developed in our laboratory,
The advantage of this technique is that the same set-up can be which has been applied successfully to measure l(T) of pure liquids
employed, irrespective of the material under test being in the solid [17], nanofluids [18], clays [19] and even-numbered paraffins [6].
or in the liquid phase. The transient hot-wire technique is nowa- The apparatus configuration and data reduction process adopted
days well established to measure l of electrically nonconducting for the present investigation were essentially the same as in the
solids, fluids and nanofluids, giving very reproducible values with preceding researchs [18,19]. The core of the apparatus is a platinum
uncertainties that can be below 1% for most of the systems [16]. wire of 50 mm diameter and about 20 cm length. Since the wires
With the exception of the critical region and the very low pressure usually break up after some weeks of continuous use and temper-
region for gases, the transient hot-wire technique has been ature cycling, three different wires with slightly different lengths,
employed successfully for wide temperature and pressure intervals. were actually employed for the measurements reported in this
For our purposes the transient hot-wire is advantageous as study. The wire is mounted in a plastic frame to keep it straight. The
compared to a flash method (that measures directly the thermal frame with the wire is placed inside a measurement cell filled with
diffusivity) or to commercial hot-disks (that require liquids to be the sample in liquid state. The temperature of the measurement cell
placed inside a vessel). is controlled by a combination of a circulation bath and a controlled
For further characterization of the samples, DSC and X-ray atmosphere chamber. For the present study, the used bath is Lauda
diffraction (XRD) tests were performed, from which more detailed ECO RE630, which permits to establish the required temperature in
information was obtained about the complex phase transition a wide range and control. Once temperature is stabilized, mea-
exhibited by these n-alkanes, that is helpful for the interpretation surements are performed by circulating through the wire an elec-
of the obtained l values. From the analysis of DSC curves, the trical current of known intensity I while acquiring readings of the
transition temperatures, the corresponding enthalpies of transi- voltage drop V(t) along the wire as a function of time. For the
tion, and the specific heat at the solid and liquid phases were electrical measurements, a Keithley 2400 source meter interfaced
determined. From XRD patterns, the structure constants of the two to a computer was employed. The theory of the hot-wire calorim-
crystalline phases exhibited by the studied n-alkanes were etry [20,21] indicates, after a short transient, a linear increase of V
estimated. with lnt
2. Experimental methods
VðtÞ ¼ a þ bln t; (1)
2.1. Materials where, in practice, a and b are two fitting parameters. Our previous
experience with this set-up [18,19] shows that, from a given run i,
The chemicals were purchased from Sigma-Aldrich and were an individual value for the thermal conductivity li can be calculated
used as supplied, without further purification. n-pentadecane by
(CH3(CH2)13 CH3, CAS 629-62-9, catalog# P3406), n-heptadecane
(CH3(CH2)15 CH3, CAS 629-78-7, catalog# 128503), and n-non-
adecane (CH3(CH2)17 CH3, CAS 629-92-5, catalog# N28906) all have Ii3 R0;i
li ¼ A ; (2)
a nominal purity of 99%. bi
2.2. Instruments where Ii is the current intensity used for the run, R0,i is the electrical
resistance measured just before switching on the current source
The DSC measurements were carried out with a DSC1 instru- (that depends on temperature at which the run is performed), and
ment (Mettler Toledo). Indium was used as standard reference for bi is the slope obtained by fitting the corresponding V(t) curve to Eq.
the calibration. The samples were sealed in aluminium pans, the (1). Finally, A in Eq. (2) represents a calibration constant that de-
masses being typically 5.8 mg for the n-pentadecane, 6.5 mg for the pends on the wire geometry and on the slope of the linear rela-
n-heptadecane and 10.1 mg for the n-nonadecane. Both heating tionship between the electrical resistance of the platinum wire and
(melting) and cooling (crystallization) curves were registered be- temperature; but not on the current Ii, neither on the (initial)
tween 258 K and 348 K with a linear increase of temperature of 2 K/ temperature at which the run is performed. In practice [18,19], A
min. All runs were performed under a constant stream of nitrogen was obtained for each one of the three wires used in this research
and at atmospheric pressure. As further explained below, transition following the ASTM-D2717 standard, carrying out preliminary
temperatures, enthalpies of transition and specific heats were ob- measurements with water and dimethylphalate covering the same
tained from the analysis of DSC curves, for which the software temperature range at which the n-alkanes were later tested.
STARe was used. Additional measurements with water after measuring the n-al-
For the XRD measurements a X'Pert PRO MPD instrument kanes are performed to check the A value and, hence, the stability of
(Panalytical) was used in the theth configuration, equipped with an the system. Notice that the constant A also includes all the sources
OxfordePhoenix low temperature camera. All measured diffracto- of systematic errors in the l measurements. Previous detailed
grams were obtained with the same range, optics, size and time analysis [18,19] yielded that the uncertainty associated with the
step. Samples were placed in a copperechromium holder under calibration procedure (and, hence, to the constant A) is ±3%. This
C. Velez et al. / International Journal of Thermal Sciences 94 (2015) 139e146 141
Table 1
Results of the analysis of DSC curves. Temperatures of phase change and corre-
sponding enthalpies of transition. Only data obtained from the analysis of heating
curves (melting) is presented.
Heating (melting)
3. Experimental results
3.1. DSC
included in these compilations. In addition, Tod in Table 1 agree well literature data [28e32]. Our current measurements are represented
with the temperatures reported by Doucet et al [11] for the OS-DS with solid circles, but they are so numerous that they appear as
phase transition obtained from XRD, i.e., 283.15 K for the n-hep- thick solid lines in Fig. 2. We observe good agreement of the current
tadecane [11] and 293.15 K for the n-nonadecane [11]. An intriguing cp measurements with literature data. It is worth quoting the lack of
fact that can be noticed in Table 1, and also quite clearly in Fig. 1, is data published in refereed scientific journals, particularly for the
the almost exact match between the OS-DS transition temperature solid phases, OS and DS. Most of the quoted literature values were
for n-heptadecane and the DS-L transition temperature for n- obtained with adiabatic calorimeters, so that they are free from the
pentadecane. Similar coincidence is detected between the OS-DS inherent limitations of the DSC method when performing cp mea-
transition temperature for n-nonadecane and the DS-L transition surements close to a phase transition.
temperature for n-heptadecane. We don't have an explanation yet To numerically report the current cp measurements, we found
for this fact, and we do believe it may be worthy of further convenient to fit the experimental points in Fig. 2 to linear tem-
investigation. perature dependence
From the analysis of DSC curves, cp can also be measured.
Actually, cp values can be obtained only for the temperature ranges cp ¼ AT þ B: (3)
that appear as almost flat in plots like Fig. 1. This means that one has
This linear fit represents the experimental data within ±2%, that
to crop the peaks corresponding to the two phase transitions.
is the estimated uncertainty of the data themselves. Hence, we
Although may be not fully evident in Fig. 1 because of the scale, it
display in Table 2 the parameters A and B obtained from these fit-
turns out that the DSC peaks corresponding to the two phase
tings for the different n-alkanes and thermodynamic phases
transitions display quite long tails, that strongly reduce the tem-
together with the corresponding temperature ranges (tempera-
perature range where reliable cp measurements by DSC are
tures in K).
possible. To alleviate this problem, we have performed DSC runs
specifically aimed to the measurement of cp with a larger linear
temperature increase of 5 K/min. In spite of this, one cannot obtain 3.2. XRD
reliable cp values inside a temperature interval of about ±12 K
around the center of the two phase transition peaks. Consequently, X-ray difractograms of the n-alkanes in the solid phases were
in no case could we obtain reliable cp values for the intermediate DS obtained as a function of temperature. For the three samples, X-ray
phase, and for the n-pentadecane we were even not able to get diffractograms were measured starting at 261 K, and up to 273 K for
reliable cp values for the OS phase. Accounting for these limitations, n-pentadecane, 291 K for n-heptadecane and 303 K for n-non-
we show in Fig. 2 the cp values that we were able to measure for the adecane. Fig. 3 shows, as an example, three difractograms obtained
three investigated n-alkanes, together with some reference for n-pentadecane at three different temperatures. The two dif-
fractograms corresponding to the solid phases display two promi-
nent peaks, while the difractogram corresponding to the liquid
phase is featureless, typical of an amorphous material.
Previous XRD studies of long-chain n-alkanes include Craig et al
[14], who used high resolution synchrotron radiation at a single
temperature for each substance. Craig et al [14] determined the
solid structure of these three n-alkanes to be orthorhombic, with
angles a¼b¼g¼90+. Similarly, Metivaud et al [10] confirm the
orthorhombic structure at lower temperatures, while finding some
orientational disorder at the crystalline II solid phase. Hence, in the
present study the X-ray diffractograms as those shown in Fig. 3
were analyzed assuming orthorhombic structure, and
Fig. 2. Isobaric specific heat capacity measured in this research (solid circles) for n-
pentadecane (top panel) n-heptadecane (middle panel) and n-nonadecane (bottom Fig. 3. Diffractograms measured for the n-pentadecane, at various temperatures as
panel). The number of points is large, so that they appear as continuous thick curves. indicated. The upper panel corresponds to the OS phase, the middle panel to the DS
Literature values, as indicated, are added with different symbols. The patterned area phase and the lower panel to the liquid phase. From the peaks displayed at solid state
corresponds, in each case, to the DS phase (between the two observed DSC peaks). the parameters of the unit cell were calculated.
C. Velez et al. / International Journal of Thermal Sciences 94 (2015) 139e146 143
Fig. 4. Unit cell parameters a (lower panel), b (middle panel) and c (upper panel) in Å, as a function of temperature, for n-pentadecane (left column) n-heptadecane (middle
column) and n-nonadecane (right column). The patterned area corresponds, in each case, to the DS phase (between the two observed DSC peaks).
determining the dimensions of the unit cell (parameters a, b and c) Larsson [13], that refer to the DS solid phase while our current data
by means of the Fullprof Suite software. The results are plotted in are for the OS phase. In addition, the measured values for the c
Fig. 4 as a function of temperature, for the three investigated n- parameter of the unit cell are consistent with the empirical corre-
alkanes. For clarity, we have patterned the temperature range lation proposed by Broadhurst [7,34].
corresponding to the disordered solid (DS) intermediate solid In addition to the literature data reported in Table 3, Doucet et al
phase, as measured by DSC. A quick look at Fig. 4 shows that the [11] also measured the unit cell parameters as a function of tem-
unit cell parameter c is, more or less, independent of temperature, perature for n-heptadecane and n-nonadecane, although they only
while parameters a and b appear to show a discontinuity at the show the results graphically. The values obtained in the present
transition between the two solid phases. Hence, structural changes study compare well with those of Doucet et al [11].
associated with the OS - DS phase change have been detected.
To quantitatively compare with reference data, we have aver- 3.3. Thermal conductivity
aged the values measured at the lower temperature phase (OS)
since Fig. 4 shows that the three parameters of the orthorhombic For each investigated n-alkane two measurement series were
unit cell are nearly independent of temperature inside this region. done. The first was from lower to higher temperature and the
Table 3 reports these averages with uncertainties obtained as second from higher to lower temperature. The reported l values are
standard deviations. Some data published in refereed scientific an average of the two series. Programmed temperatures in the
journals is also displayed in the second part of Table 3, and circulation bath ranged from 258 K to 333 K, with steps of 10 K.
reasonable agreements are found with the current values. It should Table 4 summarizes the results for l(T) including values for both the
be noted that the current values in Table 3 represent an average ordered solid phase and the liquid phase. For clarity, and for each n-
over several temperatures in the ordered solid OS region, while alkane, a horizontal line separates measurements in the solid state
literature data are for a single temperature: around 298 K for n- from measurements in the liquid state. The uncertainty indicated in
nonadecane [14,33], 264 K for n-pentadecane [14] and 278 K for n- Table 4 for the l measurements represents the random errors only,
heptadecane [14]. Poorer agreement is found with the data of and it was obtained by the same gaussian statistical analysis used
Table 3
Orthorhombic unit cell parameters for n-pentadecane, n-heptadecane and n-dodecane measured in this study (uncertainties are standard deviations) for the ordered solid
(OS) phase, and some literature reference values.
Table 4
Thermal conductivity of n-pentadecane, n-heptadecane and n-nonadecane at
various temperatures, as indicated. The uncertainty shown for the l values corre-
sponds to random errors only, a systematic error contribution estimated in ±3%
should be added. For each alkane, a horizontal line separates measurements in the
ordered solid (OS) state from measurements in the liquid state.
4. Discussion
Fig. 5. Thermal conductivity measured for n-pentadecane as a function of the tem- Fig. 7. Thermal conductivity measured for n-nonadecane as a function of the tem-
perature, together with available literature data as indicated. The patterned area cor- perature, together with available literature data as indicated. The patterned area cor-
responds to the DS phase (between the two observed DSC peaks). responds to the DS phase (between the two observed DSC peaks).
C. Velez et al. / International Journal of Thermal Sciences 94 (2015) 139e146 145
Yarbrough and Kuan [35]. Reasonable agreement with the current Acknowledgements
data is observed, particularly good for the case of n-heptadecane.
However, accounting for the larger uncertainty of the current The authors recognize the financial supports of the IþDþI
measurements for solid n-pentadecane, one can still conclude that project MAT2010-19249 (Spanish Ministry of Science and Innova-
they compare well with Yarbrough and Kuan [35] data. It should be tion) and Abengoa Water S.L.U. Partial financial support of the UCM
noticed that some of Yarbrough and Kuan [35] data, which were and Banco Santander (GR3/14, UCM Research Group “Membranes
obtained by a steady-state method, appear to refer to the disor- and Renewable Energies”) is gratefully acknowledged.
dered solid phase, for which we were unable to obtain reliable
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