A fast and low-cost dynamic calorimetric method for phase diagram estimation of binary systems


A dynamic calorimetric method based on infrared thermography has been used for the phase diagram estimation of binary systems of fatty organic materials. Its promising results make of this innovative method an interesting asset in applications with time constraints. In order to provide a calorimetry method with satisfactory performance and the lowest time consumption and cost, a test campaign is undergoing. This campaign aims at evaluating the influence of operating conditions on the performances of the method. In that frame, the phase diagrams estimated using a high-end photon detector and a low-cost microbolometer are compared. The assessment of the accuracy and reliability of phase transitions detection is made based on the study of 4 binary systems of fatty acids and fatty alcohols. Differential scanning calorimetry is used for the validation of the experimental phase diagram, and further works are identified in the light of innovative data obtained using the infrared thermography method.

This is a preview of subscription content, log in to check access.

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6


  1. 1.

    Campbell FC. Phase diagrams: understanding the basics. Cleveland: ASM International; 2012.

    Google Scholar 

  2. 2.

    Institute for Materials Research (U.S.), National Measurement Laboratory (U.S.). Office of Standard Reference Data, National Science Foundation (U.S.). Applications of phase diagrams in metallurgy and ceramics: proceedings of a Workshop Held at the National Bureau of Standards, Gaithersburg, Maryland, January 10–12, 1977.

  3. 3.

    Dubost B. Industrial applications and determination of equilibrium phase diagrams for light alloys. Progress and prospects. Rev Met Paris. 1993;90(2):195–21010.

    CAS  Article  Google Scholar 

  4. 4.

    Yang Y, Bewlay BP, Chen S, Chang YA. Application of phase diagram calculations to development of new ultra-high temperature structural materials. Trans Nonferrous Met Soc China. 2007;17(6):1396–404.

    CAS  Article  Google Scholar 

  5. 5.

    Palomo Del Barrio E, Cadoret R, Daranlot J, Achchaq F. Infrared thermography method for fast estimation of phase diagrams. Thermochim Acta. 2016;625:9–19.

    CAS  Article  Google Scholar 

  6. 6.

    Mailhé C, Duquesne M, Palomo del Barrio E, Azaiez M, Achchaq F. Phase diagrams of fatty acids as biosourced phase change materials for thermal energy storage. Appl Sci. 2019;9(6):1067.

    Article  Google Scholar 

  7. 7.

    Mailhé C, Duquesne M, Mahroug I, Palomo Del Barrio E. Improved infrared thermography method for fast estimation of complex phase diagrams. Thermochim Acta. 2019;675:84–91.

    Article  Google Scholar 

  8. 8.

    Midgley C, LMC International. The market outlook for fatty acids. ICIS Pan American Oleochemical Conference, October 2018.

  9. 9.

    OCDE, FAO. OECD-FAO Agricultural Outlook 2019–2028. Paris: OCDE Editions; 2019.

    Google Scholar 

  10. 10.

    Maximo GJ, Costa MC, Coutinho JAP, Meirelles AJA. Trends and demands in the solid–liquid equilibrium of lipidic mixtures. RSC Adv. 2014;4(60):31840–50.

    CAS  Article  Google Scholar 

  11. 11.

    Liu P, Gu X, Bian L, Peng L, He H. Capric acid/intercalated diatomite as form-stable composite phase change material for thermal energy storage. J Therm Anal Calorim. 2019;138(1):(1):359–368–368. https://doi.org/10.1139/f00-225.

    CAS  Article  Google Scholar 

  12. 12.

    Hussain SI, Kalaiselvam S. Nanoencapsulation of oleic acid phase change material with Ag2O nanoparticles-based urea formaldehyde shell for building thermal energy storage. J Therm Anal Calorim. 2019. https://doi.org/10.1007/s10973-019-08732-5.

    Article  Google Scholar 

  13. 13.

    Liu Z, Jiang L, Fu X, Zhang J, Lei J. Preparation and characterization of n-octadecane-based reversible gel as form-stable phase change materials for thermal energy storage. J Therm Anal Calorim. 2019. https://doi.org/10.1007/s10973-019-08975-2.

    Article  Google Scholar 

  14. 14.

    Gao L, Sun X, Sun B, Che D, Li S, Liu Z. Preparation and thermal properties of palmitic acid/expanded graphite/carbon fiber composite phase change materials for thermal energy storage. J Therm Anal Calorim. 2019. https://doi.org/10.1007/s10973-019-08755-y.

    Article  Google Scholar 

  15. 15.

    Vollmer M, Möllmann K-P. Infrared thermal imaging: fundamentals, research and applications. New York: Wiley; 2011. p. 2847–59–2859. https://doi.org/10.1890/04-1455.

    Google Scholar 

  16. 16.

    Syllaios A.J, Ha M, McCardel W, Schimert T. Measurement of thermal time constant of microbolometer arrays. In: Proceedings of the SPIE 5783, infrared technology and applications XXXI (31 May 2005)

  17. 17.

    Hobday AJ, Smith ADM, Stobutzki IC, Bulman C, Daley R, Dambacher JM, Deng RA, Dowdney J, Fuller M, Furlani D, Griffiths SP, Johnson D, Kenyon R, Knuckey IA, Ling SD, Pitcher R, Sainsbury KJ, Sporcic M, Smith T, Turnbull C, Walker TI, Wayte SE, Webb H, Williams A, Wise BS, Zhou S. Infrared thermography for temperature measurement and non-destructive testing. Sensors. 2014;14:12305–48–12348. https://doi.org/10.1016/j.fishres.2011.01.013.

    PubMed  Article  Google Scholar 

  18. 18.

    Boettinger WJ, Kattner UR, Moon K-W, Perepezko JH. Chapter V—DTA and heat-flux DSC measurements of alloy melting and freezing. In: Zhao JC, editor. Methods for phase diagram determination. Oxford: Elsevier Science Ltd; 2007. pp. 151–221.

    Google Scholar 

  19. 19.

    Costa MC, Sardo M, Rolemberg MP, Coutinho JAP, Meirelles AJA, Ribeiro-Claro P, et al. The solid–liquid phase diagrams of binary mixtures of consecutive, even saturated fatty acids. Chem Phys Lipid. 2007;160(2):85–97.

    CAS  Article  Google Scholar 

  20. 20.

    Maximo GJ, Carareto NDD, Costa MC, dos Santos AO, Cardoso LP, Krähenbühl MA, et al. On the solid–liquid equilibrium of binary mixtures of fatty alcohols and fatty acids. Fluid Phase Equilib. 2014;366:88–98.

    CAS  Article  Google Scholar 

  21. 21.

    Rolemberg MP. Equilibrio solido–liquido de acidos graxos e triglicerideos: determinação experimental e modelagem. 2002.

  22. 22.

    Costa MC, Sardo M, Rolemberg MP, Ribeiro-Claro P, Meirelles AJA, Coutinho JAP, et al. The solid–liquid phase diagrams of binary mixtures of consecutive, even saturated fatty acids: differing by four carbon atoms. Chem Phys Lipid. 2009;157(1):40–50.

    CAS  Article  Google Scholar 

  23. 23.

    Maximo GJ, Aquino RT, Meirelles AJA, Krähenbühl MA, Costa MC. Enhancing the description of SSLE data for binary and ternary fatty mixtures. Fluid Phase Equilib. 2016;426:119–30. https://doi.org/10.1093/conphys/cov059.

    CAS  Article  Google Scholar 

  24. 24.

    Carareto NDD, Costa MC, Meirelles AJA, Pauly J. High pressure solid-liquid equilibrium of fatty alcohols binary systems from 1-dodecanol, 1-tetradecanol, 1-hexadecanol, and 1-octadecanol. J Chem Eng Data. 2015;60(10):2966–73.

    Article  Google Scholar 

  25. 25.

    Costa MC, Rolemberg MP, Boros LAD, Krähenbühl MA, de Oliveira MG, Meirelles AJA. Solid–liquid equilibrium of binary fatty acid mixtures. J Chem Eng Data. 2007;52(1):30–6.

    CAS  Article  Google Scholar 

  26. 26.

    Gbabode G, Negrier P, Mondieig D, Moreno E, Calvet T, Cuevas-Diarte MÀ. Fatty acids polymorphism and solid-state miscibility: pentadecanoic acid–hexadecanoic acid binary system. J Alloys Compd. 2009;469(1):539–51.

    CAS  Article  Google Scholar 

  27. 27.

    Moreno E, Cordobilla R, Calvet T, Cuevas-Diarte MA, Gbabode G, Negrier P, et al. Polymorphism of even saturated carboxylic acids from n-decanoic to n-eicosanoic acid. New J Chem. 2007;31:947–57.

    CAS  Article  Google Scholar 

Download references


This work is carried out in the frame of SUDOKET project and is co-funded by the Interreg Sudoe Programme through the European Regional Development Fund (ERDF). The authors acknowledge them as well as the financial support of Region Nouvelle Aquitaine for subsidizing BioMCP project (Project-2017-1R10209-13023). We also would like to thank CNRS for promoting the I2M Bordeaux—CICe exchanges in the framework of the PICS PHASE-IR project.

Author information



Corresponding author

Correspondence to Clément Mailhé.

Additional information

Publisher's Note

Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Electronic supplementary material

Below is the link to the electronic supplementary material.

Supplementary file 1 (DOCX 83 kb)

Rights and permissions

Reprints and Permissions

About this article

Verify currency and authenticity via CrossMark

Cite this article

Mailhé, C., Duquesne, M. A fast and low-cost dynamic calorimetric method for phase diagram estimation of binary systems. J Therm Anal Calorim 143, 587–598 (2021). https://doi.org/10.1007/s10973-020-09287-6

Download citation


  • Screening
  • Infrared thermography
  • Phase diagram
  • Phase transitions
  • Fatty organic materials