A new multi-analytical procedure for radiocarbon dating of historical mortars.
ATR-FTIR
Geogenic and anthropogenic calcites
Historical mortars
Micro-Raman
Microsample preparation
Radiocarbon dating
Journal
Scientific reports
ISSN: 2045-2322
Titre abrégé: Sci Rep
Pays: England
ID NLM: 101563288
Informations de publication
Date de publication:
28 Aug 2024
28 Aug 2024
Historique:
received:
18
03
2024
accepted:
21
08
2024
medline:
31
8
2024
pubmed:
31
8
2024
entrez:
28
8
2024
Statut:
epublish
Résumé
The overarching challenge of this research is setting up a procedure to select the most appropriate fraction from complex, heterogeneous materials such as historic mortars in case of radiocarbon dating. At present, in the international community, there is not a unique and fully accepted way of mortar sample preparation to systematically obtain accurate results. With this contribution, we propose a strategy for selecting suitable mortar samples for radiocarbon dating of anthropogenic calcite in binder or lump. A four-step procedure is proposed: (I) good sampling strategies along with architectural and historical surveys; (II) mineralogical, petrographic, and chemical characterization of mortars to evaluate the feasibility of sample dating; (III) a non-destructive multi-analytical characterization of binder-rich portions to avoid geogenic calcite contamination; (IV) carbonate micro-sample preparation and accelerator mass spectrometer (AMS) measurements. The most innovative feature of the overall procedure relies on the fact that, in case of positive validation in step III, exactly the same material is treated and measured in step IV. The paper aims to apply this procedure to the ancient mortar of the Florentine historical building (Trebbio Castle), selecting micro-samples suitable for dating in natural hydraulic mortars. The discussion of the mortar dating results with the historical-archaeological hypotheses provided significant insights into the construction history of the building.
Identifiants
pubmed: 39198598
doi: 10.1038/s41598-024-70763-2
pii: 10.1038/s41598-024-70763-2
doi:
Types de publication
Journal Article
Langues
eng
Sous-ensembles de citation
IM
Pagination
19979Informations de copyright
© 2024. The Author(s).
Références
Hajdas, I. et al. Radiocarbon dating. Nat. Rev. Methods Primers 1(1), 62. https://doi.org/10.1038/s43586-021-00058-7 (2021).
doi: 10.1038/s43586-021-00058-7
Urbanová, P., Boaretto, E. & Artioli, G. The state-of-the-art of dating techniques applied to ancient mortars and binders: A review. Radiocarbon 62(3), 503–525. https://doi.org/10.1017/RDC.2020.43 (2020).
doi: 10.1017/RDC.2020.43
Hendriks, L. et al. Selective dating of paint components: Radiocarbon dating of lead white pigment. Radiocarbon 61(2), 473–493. https://doi.org/10.1017/RDC.2018.101 (2019).
doi: 10.1017/RDC.2018.101
Strunk, A., Olsen, J., Sanei, H., Rudra, A. & Larsen, N. K. Improving the reliability of bulk sediment radiocarbon dating. Quat. Sci. Rev. 242, 106442. https://doi.org/10.1016/j.quascirev.2020.106442 (2020).
doi: 10.1016/j.quascirev.2020.106442
Calandra, S. et al. Radiocarbon dating of straw fragments in the plasters of ST. Philip Church in archaeological site hierapolis of Phrygia (denizli, Turkey). Radiocarbon 65(2), 323–334. https://doi.org/10.1017/RDC.2023.20 (2023).
doi: 10.1017/RDC.2023.20
Vasco, G. et al. Mortar characterization and radiocarbon dating as support for the restoration work of the Abbey of Santa Maria di Cerrate (Lecce, South Italy). Heritage 5(4), 4161–4173. https://doi.org/10.3390/heritage5040215 (2022).
doi: 10.3390/heritage5040215
Al-Bashaireh, K. Plaster and mortar radiocarbon dating of Nabatean and Islamic structures, South Jordan. Archaeometry 55(2), 329–354. https://doi.org/10.1111/j.1475-4754.2012.00677.x (2013).
doi: 10.1111/j.1475-4754.2012.00677.x
Goedicke, C. Dating mortar by optically stimulated luminescence: A feasibility study. Geochronometria 38(1), 42–49. https://doi.org/10.2478/s13386-011-0002-0 (2011).
doi: 10.2478/s13386-011-0002-0
Panzeri, L., Maspero, F., Galli, A., Sibilia, E. & Martini, M. Luminescence and radiocarbon dating of mortars at Milano-Bicocca laboratories. Radiocarbon 62(3), 657–666. https://doi.org/10.1017/RDC.2020.6 (2020).
doi: 10.1017/RDC.2020.6
Urbanová, P. et al. The Late Antique suburban complex of Santa Giustina in Padua (North Italy): New datings and new interpretations of some architectural elements. Hortus Artium Medieval. 28, 185–200. https://doi.org/10.1484/J.HAM.5.134911 (2022).
doi: 10.1484/J.HAM.5.134911
Folk, R. & Valastro, S. Successful technique for dating of lime mortar by carbon-14. J. Field Archaeol. 3, 2 (1976).
Van Strydonck, M., Dupas, M. & Dauchot-Dehon, M. Radiocarbon dating of old mortars. PACT J. 8, 337–343 (1983).
Heinemeier, J. et al. AMS 14C dating of lime mortar. Nucl. Instrum. Methods Phys. B Beam Interact. Mater. 123(1–4), 487–495 (1997).
doi: 10.1016/S0168-583X(96)00705-7
Michalska, D., Czernik, J. & Goslar, T. Methodological aspects of mortars dating (Poznań, Poland, MODIS). Radiocarbon 59(6), 1891–1906. https://doi.org/10.1017/RDC.2017.128 (2017).
doi: 10.1017/RDC.2017.128
Hajdas, I. et al. Preparation and dating of mortar samples—Mortar Dating Intercomparison Study (MODIS). Radiocarbon 59(6), 1845–1858. https://doi.org/10.1017/RDC.2017.112 (2017).
doi: 10.1017/RDC.2017.112
Artioli, G. et al. Characterization and selection of mortar samples for radiocarbon dating in the framework of the MODIS2 intercomparison: Two compared procedures. Radiocarbon 1–14, 2024. https://doi.org/10.1017/RDC.2024.3 (2024).
doi: 10.1017/RDC.2024.3
Lichtenberger, A., Lindroos, A., Raja, R. & Heinemeier, J. Radiocarbon analysis of mortar from Roman and Byzantine water management installations in the Northwest Quarter of Jerash, Jordan. J. Archaeol. Sci. Rep. 2, 114–127. https://doi.org/10.1016/j.jasrep.2015.01.001 (2015).
doi: 10.1016/j.jasrep.2015.01.001
Fedi, M. et al. Towards micro-samples radiocarbon dating at INFN-LABEC, Florence. Nucl. Instrum. Methods Phys. Res. B Beams Interact. Mater. At. 465, 19–23. https://doi.org/10.1016/j.nimb.2019.12.020 (2020).
doi: 10.1016/j.nimb.2019.12.020
Cantisani, E. et al. The mortars of Giotto’s Bell Tower (Florence, Italy): Raw materials and technologies. Constr. Build. Mater. 267, 120801. https://doi.org/10.1016/j.conbuildmat.2020.120801 (2021).
doi: 10.1016/j.conbuildmat.2020.120801
Heinemeier, J., Ringbom, Å., Lindroos, A. & Sveinbjörnsdóttir, Á. E. Successful AMS 14C dating of non-hydraulic lime mortars from the medieval churches of the Åland Islands, Finland. Radiocarbon 52(1), 171–204. https://doi.org/10.1017/S0033822200045124 (2010).
doi: 10.1017/S0033822200045124
Ringbom, Å., Lindroos, A., Heinemeier, J. & Sonck-Koota, P. 19 years of mortar dating: Learning from experience. Radiocarbon 56(2), 619–635. https://doi.org/10.2458/56.17469 (2014).
doi: 10.2458/56.17469
Gliozzo, E., Pizzo, A. & La Russa, M. F. Mortars, plasters and pigments—research questions and sampling criteria. Archaeol. Anthropol. Sci. 13(11), 193. https://doi.org/10.1007/s12520-021-01393-2 (2021).
doi: 10.1007/s12520-021-01393-2
Boaretto, E. Dating materials in good archaeological contexts: The next challenge for radiocarbon analysis. Radiocarbon 51(1), 275–281. https://doi.org/10.1017/S0033822200033804 (2009).
doi: 10.1017/S0033822200033804
Pesce, G. L., Ball, R. J., Quarta, G. & Calcagnile, L. Identification, extraction, and preparation of reliable lime samples for 14C dating of plasters and mortars with the “pure lime lumps” technique. Radiocarbon 54(3–4), 933–942. https://doi.org/10.1017/S0033822200047573 (2012).
doi: 10.1017/S0033822200047573
Dilaria, S. et al. Phasing the history of ancient buildings through PCA on Mortars’ Mineralogical Profiles: The example of the Sarno Baths (Pompeii). Archaeometry 1–17, 2020. https://doi.org/10.1111/arcm.12746 (2020).
doi: 10.1111/arcm.12746
Miriello, D. et al. Characterisation of archaeological mortars from Pompeii (Campania, Italy) and identification of construction phases by compositional data analysis. J. Archaeol. Sci. 37(9), 2207–2223. https://doi.org/10.1016/j.jas.2010.03.019 (2010).
doi: 10.1016/j.jas.2010.03.019
Cantisani, E., Fratini, F. & Pecchioni, E. Optical and electronic microscope for minero-petrographic and microchemical studies of lime binders of ancient mortars. Minerals 12(1), 41. https://doi.org/10.3390/min12010041 (2021).
doi: 10.3390/min12010041
Artioli, G., Secco, M., & Addis, A. The Vitruvian legacy: Mortars and binders before and after the Roman world. The Contribution of Mineralogy to Cultural Heritage, Gilberto Artioli, Roberta Oberti. https://doi.org/10.1180/EMU-notes.20.4 (2019).
Arizzi, A. & Cultrone, G. Mortars and plasters—how to characterise hydraulic mortars. Archaeol. Anthropol. Sci. 13(9), 144. https://doi.org/10.1007/s12520-021-01404-2 (2021).
doi: 10.1007/s12520-021-01404-2
Pesce, G. The need for a new approach to the radiocarbon dating of historic mortars. Radiocarbon 65(5), 1017–1021. https://doi.org/10.1017/RDC.2023.92 (2023).
doi: 10.1017/RDC.2023.92
Calandra, S., Salvatici, T., Centauro, I., Cantisani, E. & Garzonio, C. A. The mortars of florence riverbanks: Raw materials and technologies of lungarni historical masonry. Appl. Sci. 12(10), 5200. https://doi.org/10.3390/app12105200 (2022).
doi: 10.3390/app12105200
Miyata, S. Anion-exchange properties of hydrotalcite-like compounds. Clays Clay Miner. 31, 305–311. https://doi.org/10.1346/CCMN.1983.0310409 (1983).
doi: 10.1346/CCMN.1983.0310409
Ponce-Antón, G., Ortega, L. A., Zuluaga, M. C., Alonso-Olazabal, A. & Solaun, J. L. Hydrotalcite and hydrocalumite in mortar binders from the medieval castle of portilla (Álava, north Spain): Accurate mineralogical control to achieve more reliable chronological ages. Minerals 8(8), 326. https://doi.org/10.3390/min8080326 (2018).
doi: 10.3390/min8080326
Sabbioni, C. et al. Atmospheric deterioration of ancient and modern hydraulic mortars. Atmos. Environ. 35(3), 539–548. https://doi.org/10.1016/S1352-2310(00)00310-1 (2001).
doi: 10.1016/S1352-2310(00)00310-1
Boynton, R. S. Chemistry and Technology of Lime and Limestone 2nd edn. (Wiley, 1980).
Bakolas, A. et al. Thermoanalytical research on traditional mortars in Venice. Thermochim. Acta 269, 817–828. https://doi.org/10.1016/0040-6031(95)02574-X (1995).
doi: 10.1016/0040-6031(95)02574-X
Moropoulou, A., Bakolas, A. & Bisbikou, K. Characterization of ancient, Byzantine and later historic mortars by thermal and X-ray diffraction techniques. Thermochim. Acta 269, 779–795. https://doi.org/10.1016/0040-6031(95)02571-5 (1995).
doi: 10.1016/0040-6031(95)02571-5
Riccardi, M. P., Lezzerini, M., Car, F., Franzini, M. & Messiga, B. Microtextural and microchemical studies of hydraulic ancient mortars: Two analytical approaches to understand pre-industrial technology processes. J. Cult. Herit. 8, 350–360. https://doi.org/10.1016/j.culher.2007.04.005 (2007).
doi: 10.1016/j.culher.2007.04.005
Marshall, J. D. Cathodoluminescence of geological materials by DJ Marshall, Unwin Hyman, 1988. https://doi.org/10.1002/gj.3350260409 (1991).
Ricci, G. et al. Integrated multi-analytical screening approach for reliable radiocarbon dating of ancient mortars. Sci. Rep. 12(1), 3339. https://doi.org/10.1038/s41598-022-07406-x (2022).
doi: 10.1038/s41598-022-07406-x
pubmed: 35228646
pmcid: 8885648
Toffolo, M. B., Ricci, G., Chapoulie, R., Caneve, L. & Kaplan-Ashiri, I. Cathodoluminescence and laser-induced fluorescence of calcium carbonate: A review of screening methods for radiocarbon dating of ancient lime mortars. Radiocarbon 62(3), 545–564. https://doi.org/10.1017/RDC.2020.21 (2020).
doi: 10.1017/RDC.2020.21
Lindroos, A., Heinemeier, J., Ringbom, Å., Braskén, M. & Sveinbjörnsdóttir, Á. Mortar dating using AMS 14C and sequential dissolution: Examples from medieval, non-hydraulic lime mortars from the Åland Islands, SW Finland. Radiocarbon 49(1), 47–67. https://doi.org/10.1017/S0033822200041898 (2007).
doi: 10.1017/S0033822200041898
Murakami, T., Hodgins, G. & Simon, A. W. Characterization of lime carbonates in plasters from Teotihuacan, Mexico: Preliminary results of cathodoluminescence and carbon isotope analyses. J. Archaeol. Sci. 40(2), 960–970. https://doi.org/10.1016/j.jas.2012.08.045 (2013).
doi: 10.1016/j.jas.2012.08.045
Chu, V., Regev, L., Weiner, S. & Boaretto, E. Differentiating between anthropogenic calcite in plaster, ash and natural calcite using infrared spectroscopy: Implications in archaeology. J. Archaeol. Sci. 35(4), 905–911. https://doi.org/10.1016/j.jas.2007.06.024 (2008).
doi: 10.1016/j.jas.2007.06.024
Regev, L., Poduska, K. M., Addadi, L., Weiner, S. & Boaretto, E. Distinguishing between calcites formed by different mechanisms using infrared 236 spectrometry: Archaeological applications. J. Archaeol. Sci. 37(12), 3022–3029. https://doi.org/10.1016/j.jas.2010.06.027 (2010).
doi: 10.1016/j.jas.2010.06.027
Toffolo, M. B., Regev, L., Dubernet, S., Lefrais, Y. & Boaretto, E. FTIR-based crystallinity assessment of aragonite–calcite mixtures in archaeological lime binders altered by diagenesis. Minerals 9(2), 121. https://doi.org/10.3390/min9020121 (2019).
doi: 10.3390/min9020121
Calandra, S. et al. Evaluation of ATR-FTIR spectroscopy for distinguishing anthropogenic and geogenic calcite. J. Phys. Conf. Ser. 2204(1), 012048. https://doi.org/10.1088/1742-6596/2204/1/012048 (2022).
doi: 10.1088/1742-6596/2204/1/012048
Surovell, T. A. & Stiner, M. C. Standardizing infrared measures of bone mineral crystallinity: An experimental approach. J. Archaeol. Sci. 28(6), 633–642. https://doi.org/10.1006/jasc.2000.0633 (2001).
doi: 10.1006/jasc.2000.0633
Seymour, L. M., Keenan-Jones, D., Zanzi, G. L., Weaver, J. C. & Masic, A. Reactive ceramic aggregates in mortars from ancient water infrastructure serving Rome and Pompeii. Cell Rep. Phys. Sci. 3, 9. https://doi.org/10.1016/j.xcrp.2022.101024 (2022).
doi: 10.1016/j.xcrp.2022.101024
Seymour, L. M. et al. Hot mixing: Mechanistic insights into the durability of ancient Roman concrete. Sci. Adv. 9(1), eadd1602. https://doi.org/10.1126/sciadv.add1602 (2023).
doi: 10.1126/sciadv.add1602
pubmed: 36608117
pmcid: 9821858
Bischoff, W. D., Sharma, S. K. & MacKenzie, F. T. Carbonate ion disorder in synthetic and biogenic magnesian calcites: A Raman spectral study. Am. Min. 70(5–6), 581–589 (1985).
Borromeo, L. et al. Raman spectroscopy as a tool for magnesium estimation in Mg- calcite. J. Raman Spectrosc. 48(7), 983–992. https://doi.org/10.1002/jrs.5156 (2017).
doi: 10.1002/jrs.5156
Zolotoyabko, E. et al. Differences between bond lengths in biogenic and geological calcite. Cryst. Growth Des. 10(3), 1207–1214. https://doi.org/10.1021/cg901195t (2010).
doi: 10.1021/cg901195t
Wehrmeister, U. et al. Amorphous, nanocrystalline and crystalline calcium carbonates in biological materials. J. Raman Spectrosc. 42(5), 926–935. https://doi.org/10.1002/jrs.2835 (2011).
doi: 10.1002/jrs.2835
Calandra, S., Conti, C., Centauro, I. & Cantisani, E. Non-destructive distinction between geogenic and anthropogenic calcite by Raman spectroscopy combined with machine learning workflow. Analyst https://doi.org/10.1039/D3AN00441D (2023).
doi: 10.1039/D3AN00441D
pubmed: 37249172
Toffolo, M. B. et al. Crystallinity assessment of anthropogenic calcites using Raman micro-spectroscopy. Sci. Rep. 13, 12971. https://doi.org/10.1038/s41598-023-39842-8 (2023).
doi: 10.1038/s41598-023-39842-8
pubmed: 37563197
pmcid: 10415260
Fedi, M. E., Cartocci, A., Manetti, M., Taccetti, F. & Mandò, P. A. The 14C AMS facility at LABEC. Florence. Nucl. Instrum. Methods Phys. Res. B Beam Interact. Mater. At. 259(1), 18–22. https://doi.org/10.1016/j.nimb.2007.01.140 (2007).
doi: 10.1016/j.nimb.2007.01.140
Arrighetti, A. Materials and building techniques in Mugello from the Late Middle Ages to the Early Modern Age; Materiali e tecniche costruttive del Mugello tra basso Medioevo e prima Età Moderna. https://doi.org/10.3989/arq.arqt.2016.001 (2017).
Brogiolo G. P. & Cagnana A. Archeologia dell’architettura. Metodi e interpretazioni (ed. All’insegna del Giglio) (2012).
Vasari, G. Le vite de' più eccellenti architetti, pittori, et scultori italiani, da Cimabue insino a' tempi nostri. Nell'edizione per i tipi di Lorenzo Torrentino, Firenze 1550 (ed. Einaudi) (2015).
Fratini, F., Cantisani, E., Pecchioni, E., Pandeli, E. & Vettori, S. Pietra Alberese: Building material and stone for lime in the Florentine Territory (Tuscany, Italy). Heritage 3(4), 1520–1538. https://doi.org/10.3390/heritage3040084 (2020).
doi: 10.3390/heritage3040084
Pavía, S. Repair mortars for masonry bridges. In Bridge and Infrastructure in Ireland, Proc. 3rdSymp, Dublin (2006).
Pecchioni, E., Fratini, F. & Cantisani, E. Atlas of the Ancient Mortars in Thin Section under Optical Microscop 2nd edn. (Nardini, 2020).
Ellerbrock, R., Stein, M. & Schaller, J. Comparing amorphous silica, short-range-ordered silicates and silicic acid species by FTIR. Sci. Rep. 12, 11708. https://doi.org/10.1038/s41598-022-15882-4 (2022).
doi: 10.1038/s41598-022-15882-4
pubmed: 35810178
pmcid: 9271067