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Thermochimica Acta
journal homepage: www.elsevier.com/locate/tca
a r t i c l e i n f o a b s t r a c t
Article history: Calorimetric techniques have become essential tools for the characterization of materials such as ceram-
Received 4 January 2013 ics, polymers, metals, drugs, foodstuffs as a function of their thermal properties. The knowledge of these
Received in revised form 4 March 2013 thermal properties (melting temperature, crystallization, glass transition, denaturation or decomposition
Accepted 12 March 2013
temperature) plays a role of great importance in the selection of the material and its manufacturing condi-
Available online 21 March 2013
tions. Despite the importance of thermal characterization there are no simple and accessible alternatives
to commercial instruments, whose main limitations are their high costs and the fragility of their consti-
Keywords:
tutive parts during operation. In this work we present the design and construction of a portable, robust
DTA
Thermal-characterization
and low cost differential thermal analysis instrument which allows for the simultaneous analysis of three
Thermal-analysis samples and it is suitable when corrosive substances are intended to be thermally characterized. This
Phase diagrams device represents an alternative to commercial devices, with applications in research and development
Instrumentation of materials in various types of industries and apt for academic training.
2013 Elsevier B.V. All rights reserved.
0040-6031/$ see front matter 2013 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.tca.2013.03.016
90 L.M. Martnez et al. / Thermochimica Acta 560 (2013) 8994
Table 1
Description of the building elements of the multi-sample DTA.
Fig. 3. Elements of the portable multi-sample-DTA: (a)USB-NI-CARD-9211with a compact DAQ chassis 9171, (b) voltage regulator, (c) aluminum-heating-block, (d) top-view
of the aluminum-heating-block with the glass sample and reference cell holders.
Fig. 4. Front panel of data acquisition and recording computer program written for the multi- simple DTA.
samples (see Fig. 5). The procedure to prepare the samples and noise of the baseline from an inert alumina sample is 0.003 a.u.
reference was described on a supplementary material of an earlier with a 95% condence interval. Therefore, the signal to noise ratio
work [9]. Glass sample cells have the advantage of allowing visual between the signals for a 10.5 mg sample of Indium, which has a
inspection of the sample before and after thermal treatment. The peak height of 0.012 a.u., and the alumina baseline is 4, which is
size of sample cell allows measuring a wide range of sample sizes an acceptable value. For a specic enthalpy of fusion of 28.66 J g1
(15150 mg). [10], this corresponds to a heat absorption of 0.3 J for this process.
2.2. Testing and calibration of the device 2.2.2. Calibration of the device with metallic indium
The portable multi-sample DTA was calibrated measuring the
To test the constructed multi sample-DTA instrument several melting point of metallic Indium. This metal is normally used as
measurements were carried out. First, a calibration was performed
with determination of melting temperature of metallic indium;
then, evaluation of base line was done to determine noise signal
ratio. The results of the melting temperature of indium were also
compared with the results obtained with a commercial device (Dia-
mond Perkin Elmer-DSC). The substance used for calibration of the
DTA was: Indium (99.99%) obtained from Sigma Aldrich. For all
measurements Aluminum Oxide, Al2 O3 (99.7%) also from Sigma
Aldrich was used as reference inert material.
established with the corresponding mass of the sample (see Fig. 8b).
A coefcient of determination, r2 , of 0.9721 was obtained, suggest-
ing a good correlation between the DTA signal and the amount of
the sample.
Fig. 8. DTA thermograms showing the endothermic melting process of indium samples of different masses. On the right side, the area of each melting peak was calculated
and plotted against the corresponding mass of the sample to nd a linear correlation.
L.M. Martnez et al. / Thermochimica Acta 560 (2013) 8994 93
References