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Estimation of the linseed oil content in historic lime mortar

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Abstract

Vegetable oils (e.g. linseed or tung) were used as lime mortar admixtures in order to increase the mortar durability (due to the water repealing effect) and/or to prolong the mortar’s workability. The present paper aims to investigate the possibilities of thermal analysis to estimate the linseed oil content in a historic mortar. A set of model mortars containing Ca(OH)2, CaCO3 and variable amount of linseed oil was studied by methods usually used for mortars characterization: thermogravimetry with evolved gas analysis by mass spectroscopy (TG EGA-MS), FTIR spectroscopy (Fourier transform infrared spectroscopy) and XRD (powder X-ray diffraction). Oil admixed in lime mortar undergoes two principal transformations: saponification to Ca carboxylates and polymerization (drying). The products of the oil transformation are thermally decomposing during the thermal analysis experiment, but unfortunately in the same temperature range as Ca(OH)2—common mortar component—does. A calculation procedure which enables to determine content of both Ca(OH)2 and “oil products” on base of thermogravimetry was proposed. As an alternative, an estimation of oil content based on EGA-MS results for m/z 95 ion was developed. Finally, total organic carbon (TOC) may be also used if any other organics are not present. These three approaches were used for the oil content estimation in the sample of historic mosaic mortar. The result obtained by TG EGA-MS approach was found to be the most realistic.

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References

  1. Özen S, Altun MG, Mardani-Aghabaglou A, Ramyar K. Effect of main and side chain length change of polycarboxylate-ether-based water-reducing admixtures on the fresh state and mechanical properties of cementitious systems. Struct Concr. 2021. https://doi.org/10.1002/suco.201900489.

    Article  Google Scholar 

  2. Nogueira R, Ferreira Pinto AP, Gomes A. Design and behavior of traditional lime-based plasters and renders. Review and critical appraisal of strengths and weaknesses. Cem Concr Compos. 2018. https://doi.org/10.1016/j.cemconcomp.2018.03.005.

    Article  Google Scholar 

  3. Kuckova S, Rambouskova G, Junkova P, Santrucek J, Cejnar P, Smirnova TA, Novotny O, Hynek R. Analysis of protein additives degradation in aged mortars using mass spectrometry and principal component analysis. Constr Build Mat. 2021. https://doi.org/10.1016/j.conbuildmat.2021.123124.

    Article  Google Scholar 

  4. Fang S, Zhang K, Zhang H, Zhang B. A study of traditional blood lime mortar for restoration of ancient buildings. Cem Concr Res. 2015. https://doi.org/10.1016/j.cemconres.2015.06.006.

    Article  Google Scholar 

  5. Izaguirre A, Lanas J, Álvarez JI. Behaviour of a starch as a viscosity modifier for aerial lime-based mortars. Carbohydr Polym. 2010. https://doi.org/10.1016/j.carbpol.2009.11.010.

    Article  Google Scholar 

  6. Yang T, Ma X, Zhang B, Zhang H. Investigations into the function of sticky rice on the microstructures of hydrated lime putties. Constr Build Mater. 2016. https://doi.org/10.1016/j.conbuildmat.2015.10.183.

    Article  Google Scholar 

  7. Vitruvius. Ten Books on Architecture. Cambridge University Press, Cambridge.1999.

  8. Nunes C, Slížková Z, Křivánková D. Lime-based mortars with linseed oil: sodium chloride resistance assessment and characterization of the degraded material. Period Miner. 2013. https://doi.org/10.2451/2013PM0024.

    Article  Google Scholar 

  9. Papayianni I, Pachta V, Stefanidou M. Analysis of ancient mortars and design of compatible repair mortars: The case study of Odeion of the archaeological site of Dion. Con Build Mat. 2013. https://doi.org/10.1016/j.conbuildmat.2012.09.086

  10. Nunes C, Slížková Z. Freezing and thawing resistance of aerial lime mortar with metakaolin and a traditional water-repellent admixture. Constr Build Mater. 2016. https://doi.org/10.1016/j.conbuildmat.2016.04.029.

    Article  Google Scholar 

  11. Bauerová P, Reiterman P, Davidová V, Vejmelková E, Kracík Štorkánová M, Keppert M. Lime mortars with linseed oil: engineering properties and durability. Rom J Mater. 2021;51:239–46.

    Google Scholar 

  12. Fiori C, Vandini M, Prati S, Chiavari G. Vaterite in the mortars of a mosaic in the Saint Peter basilica, Vatican (Rome). J Cult Herit. 2008. https://doi.org/10.1016/j.culher.2008.07.011.

    Article  Google Scholar 

  13. La GE. Mosaïque. Paris: Quantin Editeur; 1880.

    Google Scholar 

  14. Bauerová P, Reiterman P, Kracík Štorkánová M, Keppert M. Mechanical properties of reporduced historic mosiac mortar. Solid State Phenom. 2021. https://doi.org/10.4028/www.scientific.net/SSP.325.86.

    Article  Google Scholar 

  15. Zhao P, Jackson MD, Zhang Y, Li G, Monteiro PJM, Yang L. Material characteristics of ancient Chinese lime binder and experimental reproductions with organic admixtures. Constr Build Mater. 2015. https://doi.org/10.1016/j.conbuildmat.2015.03.065.

    Article  Google Scholar 

  16. Wang S, Yao W, Lu Z, Wang S, Li B, Liu B. Characterization and durability assessment of fibre-reinforced tung oil lime putties for restoration. J Buil Eng. 2021. https://doi.org/10.1016/j.jobe.2021.102241.

    Article  Google Scholar 

  17. Izaguirre A, Lanas J, Álvarez JI. Effect of water-repellent admixtures on the behaviour of aerial lime-based mortars. Cem Concr Res. 2009. https://doi.org/10.1016/j.cemconres.2009.07.026.

    Article  Google Scholar 

  18. Middendorf B, Hughes JJ, Callebaut K, Baronio G, Papayanni I. Investigative methods for the characterisation of historic mortars—Part 1: Mineralogical characterisation. Mater Struct. 2005. https://doi.org/10.1007/BF02479289.

    Article  Google Scholar 

  19. Middendorf B, Hughes JJ, Callebaut K, Baronio G, Papayanni I. Investigative methods for the characterisation of historic mortars—part 2: Chemical characterisation. Mater Struct. 2005. https://doi.org/10.1007/BF02479290.

    Article  Google Scholar 

  20. Fang SQ, Zhang H, Zhang BJ, Zheng Y. The identification of organic additives in traditional lime mortar. J Cult Herit. 2014. https://doi.org/10.1016/j.culher.2013.04.001.

    Article  Google Scholar 

  21. Krizova I, Schultz J, Nemec I, Cabala R, Hynek R, Kuckova S. Comparison of analytical tools appropriate for identification of proteinaceous additives in historical mortars. Anal Bioanal Chem. 2018. https://doi.org/10.1007/s00216-017-0709-8.

    Article  Google Scholar 

  22. Guasch-Ferré N, Prada Pérez JL, de Árgedos V, Pascual ML, Osete-Cortina L, Doménech-Carbó MT. Polysaccharide remains in Maya mural paintings: is it an evidence of the use of plant gums as binding medium of pigments and additive in the mortar? Sci Tech Archaeol Res. 2020. https://doi.org/10.1080/20548923.2020.1720377.

    Article  Google Scholar 

  23. Luxán MP, Dorrego F, Laborde A. Ancient gypsum mortars from St. Engracia (Zaragoza, Spain): characterization, identification of additives and treatments. Cem Concr Res. 1995. https://doi.org/10.1016/0008-8846(95)00171-9.

    Article  Google Scholar 

  24. Bauerová P, Kracík Štorkánová M, Mácová P, Scheinherrová L, Keppert M. Searching for common technological features of 19th–20th-century mosaic mortars ascribed to the Neuhauser company. Archeometry. 2021. https://doi.org/10.1111/arcm.12678.

    Article  Google Scholar 

  25. Vlase D, Codruta M, Vlase G, Lazau R, Vlase T. Comparative analyses of roman mortars belonging to different ancient periods from Drobeta-Turnu Severin region. J Therm Anal Calorim. 2020. https://doi.org/10.1007/s10973-020-09917-z.

    Article  Google Scholar 

  26. Nunes C, Viani A, Ševčík R. Microstructural analysis of lime paste with the addition of linseed oil, stand oil, and rapeseed oil. Constr Build Mater. 2020. https://doi.org/10.1016/j.conbuildmat.2019.117780.

    Article  Google Scholar 

  27. Döbelin N, Kleeberg R. Profex: a graphical user interface for the Rietveld refinement program BGMN. J Appl Crystallogr. 2015. https://doi.org/10.1107/S1600576715014685.

    Article  Google Scholar 

  28. Mjøs SA. The prediction of fatty acid structure from selected ions in electron impact mass spectra of fatty acid methyl esters. Eur Lipid Sci Technol. 2004. https://doi.org/10.1002/ejlt.200401013.

    Article  Google Scholar 

  29. Orsini S, Parlanti F, Bonaduce I. Analytical pyrolysis of proteins in samples from artistic and archaeological objects. J Anal Appl Pyrolysis. 2017. https://doi.org/10.1016/j.jaap.2016.12.017.

    Article  Google Scholar 

  30. de Viguerie L, Payard PA, Portero E, Walter P, Cotte M. The drying of linseed oil investigated by FOURIER transform infrared spectroscopy: historical recipes and influence of lead compounds. Prog Org Coat. 2016. https://doi.org/10.1016/j.porgcoat.2015.12.010.

    Article  Google Scholar 

  31. Xu B, Poduska KM. Linking crystal structure with temperature-sensitive vibrational modes in calcium carbonate minerals. Phys Chem Chem Phys. 2014. https://doi.org/10.1039/c4cp01772b.

    Article  Google Scholar 

  32. Švarcová S, Kočí E, Plocek J, Zhankina A, Hradilová J, Bezdička P. Saponification in egg yolk-based tempera paintings with lead-tin yellow type I. J Cult Herit. 2019. https://doi.org/10.1016/j.culher.2018.12.004.

    Article  Google Scholar 

  33. Rodriguez LM, Fernandez MB, Perez EE, Crapiste GH. Performance of green solvents in the extraction of sunflower oil from enzyme-treated collets. Eur J Lipid Sci Tech. 2021. https://doi.org/10.1002/ejlt.202000132.

    Article  Google Scholar 

  34. van der Weerd J, van Loon A, Boon JJ. FTIR studies of the effects of pigments on the aging of oil. Stud Conserv. 2005. https://doi.org/10.1179/sic.2005.50.1.3

  35. Schönemann A, Edwards HGM. Raman and FTIR microspectroscopic study of the alteration of Chinese tung oil and related drying oils during ageing. Anal Bioanal Chem. 2011. https://doi.org/10.1007/s00216-011-4855-0.

    Article  Google Scholar 

  36. Honzíček J. Curing of air-drying paints: a critical review. Ind Eng Chem Res. 2019. https://doi.org/10.1021/acs.iecr.9b02567.

    Article  Google Scholar 

  37. Poulenat G, Sentenac S, Mouloungul Z. Fourier-transform infrared spectra of fatty acid salts—kinetics of high-oleic sunflower oil saponification. J Surfactants Deterg. 2003. https://doi.org/10.1007/s11743-003-0274-1.

    Article  Google Scholar 

  38. Barannikov R, Kočí E, Bezdička P, Kobera L, Mahun A, Rohlíček J, Plocek J, Švarcová S. Long-chain mercury carboxylates relevant to saponification in oil and tempera paintings: XRPD and ssNMR complementary study of their crystal structures. Dalton Trans. 2022. https://doi.org/10.1039/d1dt04160f.

    Article  Google Scholar 

  39. Seniha Grüner F, Yagci Y, Tuncer EA. Polymers from triglyceride oils. Prog Polym Sci. 2006. https://doi.org/10.1016/j.progpolymsci.2006.07.001.

    Article  Google Scholar 

  40. Falzone G, Mehdipour I, Neithalath N, Bauchy M, Simonetti D, Sant G. New insights into the mechanisms of carbon dioxide mineralization by portlandite. AICHE J. 2021. https://doi.org/10.1002/aic.17160.

    Article  Google Scholar 

  41. Kočí E, Rohlíček J, Kobera L, Plocek J, Švarcová S, Bezdička P. Mixed lead carboxylates relevant to soap formation in oil and tempera paintings: the study of the crystal structure by complementary XRPD and ssNMR. Dalton Trans. 2019. https://doi.org/10.1039/c9dt02040c.

    Article  Google Scholar 

  42. Garrappa S, Hradil D, Hradilová J, Kočí E, Pech M, Bezdička P, Švarcová S. Non-invasive identification of lead soaps in painted miniatures. Anal Bioanal Chem. 2021. https://doi.org/10.1007/s00216-020-02998-7.

    Article  Google Scholar 

  43. Rampazzi L, Colombini MP, Conti C, Corti C, Lluveras-Tenorio A, Sansonetti A, Zanaboni M. Technology of medieval mortars: an investigation into the use of organic additives. Archaeometry. 2015. https://doi.org/10.1111/arcm.12155.

    Article  Google Scholar 

  44. Cígler Žofková D, Frankl J, Frankeová D. Use of thermal analysis for the detection of calcium oxalate in selected forms of plastering exposed to the effects of Serpula Lacrymans. Acta Polytechnica. 2021. https://doi.org/10.14311/AP.2021.61.0511.

    Article  Google Scholar 

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Acknowledgements

The paper was supported by the Czech Science Foundation under the project no. 18-13525S and by the Czech Technical University in Prague under the project no. SGS22/137/OHK1/3T/11. This research was also supported by the Czech Academy of Sciences in the framework “Strategy AV21—Program No. 23. City as a Laboratory of Change; Construction, Historical Heritage and Place for Safe and Quality Life”.

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Authors and Affiliations

  1. Department of Materials Engineering and Chemistry, Faculty of Civil Engineering, Czech Technical University in Prague, Thákurova 7, 166 29, Praha 6, Czech Republic

    Pavla Bauerová, Eva Vejmelková & Martin Keppert

  2. Institute of Theoretical and Applied Mechanics of Czech Academy of Sciences, Prosecká 809/76, 190 00, Prague 9, Czech Republic

    Pavla Bauerová & Petra Mácová

  3. Art and Craft Mozaika, Z.S., Kapitulní 103/19, 252 62, Únětice, Czech Republic

    Magdalena Kracík-Štorkánová

  4. University Centre for Energy Efficient Buildings, Czech Technical University in Prague, Třinecká 1024, 273 43, Buštěhrad, Czech Republic

    Pavel Reiterman

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PB, MK-Š, and MK were involved in conceptualization.MK was involved in formal analysis, resources, and writing—review & editing. PB, PM, PR, and EV were involved in investigation. PB and MK were involved in writing—original draft.

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Correspondence to Martin Keppert.

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Bauerová, P., Kracík-Štorkánová, M., Mácová, P. et al. Estimation of the linseed oil content in historic lime mortar. J Therm Anal Calorim 148, 697–709 (2023). https://doi.org/10.1007/s10973-022-11792-9

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