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Dilaria S., Secco M., Bonetto J., Artioli G. 2019 - Technical analysis on materials and characteristics of mortar-based compounds in Roman and Late antique Aquileia (Udine, Italy). A preliminary report of the results

2019, 5 th Historic Mortars Conference – 19-21 June 2019 – Pamplona, Spain

In the present paper we report the preliminary results of an ongoing research focused on the investigation of Roman mortars and concretes employed in Aquileia from Roman to Early Medieval Age (II century BC – VI century AD). More than 250 samples have been collected from buildings spread all over of the town, with different chronologies of construction and different functions. Material characterization was achieved throughout a multi-analytical approach comprising optical microscopy (OM), X-Ray powder diffraction (XRPD) and Scanning Electron Microscopy-Energy Dispersive microanalysis (SEM-EDS). Analytical data have been strictly crosschecked in relation with the chronology and purpose of the structure from which mortars have been collected from. The preliminary results we obtained are providing intriguing outcomes: we observed a high specialization on “recipes” in relation to the function of mortars and concretes, but also chronology of production appears to have an important role in the composition of mortar-based compounds. Such an extensive sampling is giving valuable insights to decipher the relations among crafts and artisans in ancient construction and decorative activities.

Proceedings PRO 130 Proceedings of the 5th Historic Mortars Conference Edited by José Ignacio Álvarez, José María Fernández, Íñigo Navarro, Adrián Durán, Rafael Sirera RILEM Publications S.A.R.L. 5th Historic Mortars Conference 5th Historic Mortars Conference 19-21 June 2019 Pamplona, Spain Edited by José Ignacio Álvarez, José María Fernández, Íñigo Navarro, Adrián Durán, Rafael Sirera RILEM Publications S.A.R.L. 5th Historic Mortars Conference – 19-21 June 2019 – Pamplona, Spain Published by RILEM Publications S.A.R.L. 4 avenue du Recteur Poincaré 75016 Paris - France Tel : + 33 1 42 24 64 46 Fax : + 33 9 70 29 51 20 http://www.rilem.net E-mail: dg@rilem.net  2019 RILEM – Tous droits réservés. ISBN: 978-2-35158-221-3 e-ISBN: 978-2-35158-222-0 Publisher's note: this book has been produced from electronic files provided by the individual contributors. The publisher makes no representation, express or implied, with regard to the accuracy of the information contained in this book and cannot accept any legal responsibility or liability for any errors or omissions that may be made. All titles published by RILEM Publications are under copyright protection; said copyrights being the property of their respective holders. All Rights Reserved. No part of any book may be reproduced or transmitted in any form or by any means, graphic, electronic, or mechanical, including photocopying, recording, taping, or by any information storage or retrieval system, without the permission in writing from the publisher. RILEM, The International Union of Laboratories and Experts in Construction Materials, Systems and Structures, is a non profit-making, non-governmental technical association whose vocation is to contribute to progress in the construction sciences, techniques and industries, essentially by means of the communication it fosters between research and practice. RILEM’s activity therefore aims at developing the knowledge of properties of materials and performance of structures, at defining the means for their assessment in laboratory and service conditions and at unifying measurement and testing methods used with this objective. RILEM was founded in 1947, and has a membership of over 900 in some 70 countries. It forms an institutional framework for co-operation by experts to: • optimise and harmonise test methods for measuring properties and performance of building and civil engineering materials and structures under laboratory and service environments, • prepare technical recommendations for testing methods, • prepare state-of-the-art reports to identify further research needs, • collaborate with national or international associations in realising these objectives. RILEM members include the leading building research and testing laboratories around the world, industrial research, manufacturing and contracting interests, as well as a significant number of individual members from industry and universities. RILEM’s focus is on construction materials and their use in building and civil engineering structures, covering all phases of the building process from manufacture to use and recycling of materials. RILEM meets these objectives through the work of its technical committees. Symposia, workshops and seminars are organised to facilitate the exchange of information and dissemination of knowledge. RILEM’s primary output consists of technical recommendations. RILEM also publishes the journal Materials and Structures which provides a further avenue for reporting the work of its committees. Many other publications, in the form of reports, monographs, symposia and workshop proceedings are produced. II 5th Historic Mortars Conference – 19-21 June 2019 – Pamplona, Spain RILEM Publications The following list is presenting the global offer of RILEM Publications, sorted by series. Each publication is available in printed version and/or in online version. RILEM PROCEEDINGS (PRO) PRO 1: Durability of High Performance Concrete (ISBN: 2-912143-03-9); Ed. H. Sommer PRO 2: Chloride Penetration into Concrete (ISBN: 2-912143-00-04); Eds. L.-O. Nilsson and J.-P. Ollivier PRO 3: Evaluation and Strengthening of Existing Masonry Structures (ISBN: 2-912143-02-0); Eds. L. Binda and C. Modena PRO 4: Concrete: From Material to Structure (ISBN: 2-912143-04-7); Eds. J.-P. Bournazel and Y. Malier PRO 5: The Role of Admixtures in High Performance Concrete (ISBN: 2-912143-05-5); Eds. J. G. Cabrera and R. Rivera-Villarreal PRO 6: High Performance Fiber Reinforced Cement Composites - HPFRCC 3 (ISBN: 2-912143-06-3); Eds. H. W. Reinhardt and A. E. Naaman PRO 7: 1st International RILEM Symposium on Self-Compacting Concrete (ISBN: 2-912143-098); Eds. Å. Skarendahl and Ö. Petersson PRO 8: International RILEM Symposium on Timber Engineering (ISBN: 2-912143-10-1); Ed. L. Boström PRO 9: 2nd International RILEM Symposium on Adhesion between Polymers and Concrete ISAP ’99 (ISBN: 2-912143-11-X); Eds. Y. Ohama and M. Puterman PRO 10: 3rd International RILEM Symposium on Durability of Building and Construction Sealants (ISBN: 2-912143-13-6); Eds. A. T. Wolf PRO 11: 4th International RILEM Conference on Reflective Cracking in Pavements (ISBN: 2-912143-14-4); Eds. A. O. Abd El Halim, D. A. Taylor and El H. H. Mohamed PRO 12: International RILEM Workshop on Historic Mortars: Characteristics and Tests (ISBN: 2-912143-15-2); Eds. P. Bartos, C. Groot and J. J. Hughes PRO 13: 2nd International RILEM Symposium on Hydration and Setting (ISBN: 2-912143-160); Ed. A. Nonat PRO 14: Integrated Life-Cycle Design of Materials and Structures - ILCDES 2000 (ISBN: 951-758-408-3); (ISSN: 0356-9403); Ed. S. Sarja PRO 15: Fifth RILEM Symposium on Fibre-Reinforced Concretes (FRC) - BEFIB’2000 (ISBN: 2-912143-18-7); Eds. P. Rossi and G. Chanvillard PRO 16: Life Prediction and Management of Concrete Structures (ISBN: 2-912143-19-5); Ed. D. Naus PRO 17: Shrinkage of Concrete – Shrinkage 2000 (ISBN: 2-912143-20-9); Eds. V. Baroghel-Bouny and P.-C. Aïtcin PRO 18: Measurement and Interpretation of the On-Site Corrosion Rate (ISBN: 2-912143-21-7); Eds. C. Andrade, C. Alonso, J. Fullea, J. Polimon and J. Rodriguez PRO 19: Testing and Modelling the Chloride Ingress into Concrete (ISBN: 2-912143-22-5); Eds. C. Andrade and J. Kropp III 5th Historic Mortars Conference – 19-21 June 2019 – Pamplona, Spain PRO 20: 1st International RILEM Workshop on Microbial Impacts on Building Materials (CD 02) (e-ISBN 978-2-35158-013-4); Ed. M. Ribas Silva PRO 21: International RILEM Symposium on Connections between Steel and Concrete (ISBN: 2-912143-25-X); Ed. R. Eligehausen PRO 22: International RILEM Symposium on Joints in Timber Structures (ISBN: 2-912143-28-4); Eds. S. Aicher and H.-W. Reinhardt PRO 23: International RILEM Conference on Early Age Cracking in Cementitious Systems (ISBN: 2-912143-29-2); Eds. K. Kovler and A. Bentur PRO 24: 2nd International RILEM Workshop on Frost Resistance of Concrete (ISBN: 2-912143-30-6); Eds. M. J. Setzer, R. Auberg and H.-J. Keck PRO 25: International RILEM Workshop on Frost Damage in Concrete (ISBN: 2-912143-31-4); Eds. D. J. Janssen, M. J. Setzer and M. B. Snyder PRO 26: International RILEM Workshop on On-Site Control and Evaluation of Masonry Structures (ISBN: 2-912143-34-9); Eds. L. Binda and R. C. de Vekey PRO 27: International RILEM Symposium on Building Joint Sealants (CD03); Ed. A. T. Wolf PRO 28: 6th International RILEM Symposium on Performance Testing and Evaluation of Bituminous Materials - PTEBM’03 (ISBN: 2-912143-35-7; e-ISBN: 978-2-912143-77-8); Ed. M. N. Partl PRO 29: 2nd International RILEM Workshop on Life Prediction and Ageing Management of Concrete Structures (ISBN: 2-912143-36-5); Ed. D. J. Naus PRO 30: 4th International RILEM Workshop on High Performance Fiber Reinforced Cement Composites - HPFRCC 4 (ISBN: 2-912143-37-3); Eds. A. E. Naaman and H. W. Reinhardt PRO 31: International RILEM Workshop on Test and Design Methods for Steel Fibre Reinforced Concrete: Background and Experiences (ISBN: 2-912143-38-1); Eds. B. Schnütgen and L. Vandewalle PRO 32: International Conference on Advances in Concrete and Structures 2 vol. (ISBN (set): 2-912143-41-1); Eds. Ying-shu Yuan, Surendra P. Shah and Heng-lin Lü PRO 33: 3rd International Symposium on Self-Compacting Concrete (ISBN: 2-912143-42-X); Eds. Ó. Wallevik and I. Níelsson PRO 34: International RILEM Conference on Microbial Impact on Building Materials (ISBN: 2-912143-43-8); Ed. M. Ribas Silva PRO 35: International RILEM TC 186-ISA on Internal Sulfate Attack and Delayed Ettringite Formation (ISBN: 2-912143-44-6); Eds. K. Scrivener and J. Skalny PRO 36: International RILEM Symposium on Concrete Science and Engineering – A Tribute to Arnon Bentur (ISBN: 2-912143-46-2); Eds. K. Kovler, J. Marchand, S. Mindess and J. Weiss PRO 37: 5th International RILEM Conference on Cracking in Pavements – Mitigation, Risk Assessment and Prevention (ISBN: 2-912143-47-0); Eds. C. Petit, I. Al-Qadi and A. Millien PRO 38: 3rd International RILEM Workshop on Testing and Modelling the Chloride Ingress into Concrete (ISBN: 2-912143-48-9); Eds. C. Andrade and J. Kropp PRO 39: 6th International RILEM Symposium on Fibre-Reinforced Concretes - BEFIB 2004 (ISBN: 2-912143-51-9); Eds. M. Di Prisco, R. Felicetti and G. A. Plizzari PRO 40: International RILEM Conference on the Use of Recycled Materials in Buildings and Structures (ISBN: 2-912143-52-7); Eds. E. Vázquez, Ch. F. Hendriks and G. M. T. Janssen PRO 41: RILEM International Symposium on Environment-Conscious Materials and Systems for Sustainable Development (ISBN: 2-912143-55-1); Eds. N. Kashino and Y. Ohama IV 5th Historic Mortars Conference – 19-21 June 2019 – Pamplona, Spain PRO 42: SCC’2005 - China: 1st International Symposium on Design, Performance and Use of Self-Consolidating Concrete (ISBN: 2-912143-61-6); Eds. Zhiwu Yu, Caijun Shi, Kamal Henri Khayat and Youjun Xie PRO 43: International RILEM Workshop on Bonded Concrete Overlays (e-ISBN: 2-912143-837); Eds. J. L. Granju and J. Silfwerbrand PRO 44: 2nd International RILEM Workshop on Microbial Impacts on Building Materials (CD11) (e-ISBN: 2-912143-84-5); Ed. M. Ribas Silva PRO 45: 2nd International Symposium on Nanotechnology in Construction, Bilbao (ISBN: 2-912143-87-X); Eds. Peter J. M. Bartos, Yolanda de Miguel and Antonio Porro PRO 46: ConcreteLife’06 - International RILEM-JCI Seminar on Concrete Durability and Service Life Planning: Curing, Crack Control, Performance in Harsh Environments (ISBN: 2-912143-89-6); Ed. K. Kovler PRO 47: International RILEM Workshop on Performance Based Evaluation and Indicators for Concrete Durability (ISBN: 978-2-912143-95-2); Eds. V. Baroghel-Bouny, C. Andrade, R. Torrent and K. Scrivener PRO 48: 1st International RILEM Symposium on Advances in Concrete through Science and Engineering (e-ISBN: 2-912143-92-6); Eds. J. Weiss, K. Kovler, J. Marchand, and S. Mindess PRO 49: International RILEM Workshop on High Performance Fiber Reinforced Cementitious Composites in Structural Applications (ISBN: 2-912143-93-4); Eds. G. Fischer and V.C. Li PRO 50: 1st International RILEM Symposium on Textile Reinforced Concrete (ISBN: 2-912143-97-7); Eds. Josef Hegger, Wolfgang Brameshuber and Norbert Will PRO 51: 2nd International Symposium on Advances in Concrete through Science and Engineering (ISBN: 2-35158-003-6; e-ISBN: 2-35158-002-8); Eds. J. Marchand, B. Bissonnette, R. Gagné, M. Jolin and F. Paradis PRO 52: Volume Changes of Hardening Concrete: Testing and Mitigation (ISBN: 2-35158-0044; e-ISBN: 2-35158-005-2); Eds. O. M. Jensen, P. Lura and K. Kovler PRO 53: High Performance Fiber Reinforced Cement Composites - HPFRCC5 (ISBN: 978-2-35158-046-2); Eds. H. W. Reinhardt and A. E. Naaman PRO 54: 5th International RILEM Symposium on Self-Compacting Concrete (ISBN: 978-2-35158-047-9); Eds. G. De Schutter and V. Boel PRO 55: International RILEM Symposium Photocatalysis, Environment and Construction Materials (ISBN: 978-2-35158-056-1); Eds. P. Baglioni and L. Cassar PRO56: International RILEM Workshop on Integral Service Life Modelling of Concrete Structures (ISBN 978-2-35158-058-5); Eds. R. M. Ferreira, J. Gulikers and C. Andrade PRO57: RILEM Workshop on Performance of cement-based materials in aggressive aqueous environments (e-ISBN: 978-2-35158-059-2); Ed. N. De Belie PRO58: International RILEM Symposium on Concrete Modelling - CONMOD’08 (ISBN: 978-2-35158-060-8); Eds. E. Schlangen and G. De Schutter PRO 59: International RILEM Conference on On Site Assessment of Concrete, Masonry and Timber Structures - SACoMaTiS 2008 (ISBN set: 978-2-35158-061-5); Eds. L. Binda, M. di Prisco and R. Felicetti PRO 60: Seventh RILEM International Symposium on Fibre Reinforced Concrete: Design and Applications - BEFIB 2008 (ISBN: 978-2-35158-064-6); Ed. R. Gettu PRO 61: 1st International Conference on Microstructure Related Durability of Cementitious Composites 2 vol., (ISBN: 978-2-35158-065-3); Eds. W. Sun, K. van Breugel, C. Miao, G. Ye and H. Chen V 5th Historic Mortars Conference – 19-21 June 2019 – Pamplona, Spain PRO 62: NSF/ RILEM Workshop: In-situ Evaluation of Historic Wood and Masonry Structures (e-ISBN: 978-2-35158-068-4); Eds. B. Kasal, R. Anthony and M. Drdácký PRO 63: Concrete in Aggressive Aqueous Environments: Performance, Testing and Modelling, 2 vol., (ISBN: 978-2-35158-071-4); Eds. M. G. Alexander and A. Bertron PRO 64: Long Term Performance of Cementitious Barriers and Reinforced Concrete in Nuclear Power Plants and Waste Management - NUCPERF 2009 (ISBN: 978-2-35158-072-1); Eds. V. L’Hostis, R. Gens, C. Gallé PRO 65: Design Performance and Use of Self-consolidating Concrete - SCC’2009 (ISBN: 978-2-35158-073-8); Eds. C. Shi, Z. Yu, K. H. Khayat and P. Yan PRO 66: 2nd International RILEM Workshop on Concrete Durability and Service Life Planning ConcreteLife’09 (ISBN: 978-2-35158-074-5); Ed. K. Kovler PRO 67: Repairs Mortars for Historic Masonry (e-ISBN: 978-2-35158-083-7); Ed. C. Groot PRO 68: Proceedings of the 3rd International RILEM Symposium on ‘Rheology of Cement Suspensions such as Fresh Concrete (ISBN 978-2-35158-091-2); Eds. O. H. Wallevik, S. Kubens and S. Oesterheld PRO 69: 3rd International PhD Student Workshop on ‘Modelling the Durability of Reinforced Concrete (ISBN: 978-2-35158-095-0); Eds. R. M. Ferreira, J. Gulikers and C. Andrade PRO 70: 2nd International Conference on ‘Service Life Design for Infrastructure’ (ISBN set: 9782-35158-096-7, e-ISBN: 978-2-35158-097-4); Ed. K. van Breugel, G. Ye and Y. Yuan PRO 71: Advances in Civil Engineering Materials - The 50-year Teaching Anniversary of Prof. Sun Wei’ (ISBN: 978-2-35158-098-1; e-ISBN: 978-2-35158-099-8); Eds. C. Miao, G. Ye, and H. Chen PRO 72: First International Conference on ‘Advances in Chemically-Activated Materials – CAM’2010’ (2010), 264 pp, ISBN: 978-2-35158-101-8; e-ISBN: 978-2-35158-115-5, Eds. Caijun Shi and Xiaodong Shen PRO 73: 2nd International Conference on ‘Waste Engineering and Management - ICWEM 2010’ (2010), 894 pp, ISBN: 978-2-35158-102-5; e-ISBN: 978-2-35158-103-2, Eds. J. Zh. Xiao, Y. Zhang, M. S. Cheung and R. Chu PRO 74: International RILEM Conference on ‘Use of Superabsorsorbent Polymers and Other New Addditives in Concrete’ (2010) 374 pp., ISBN: 978-2-35158-104-9; e-ISBN: 978-2-35158105-6; Eds. O.M. Jensen, M.T. Hasholt, and S. Laustsen PRO 75: International Conference on ‘Material Science - 2nd ICTRC - Textile Reinforced Concrete - Theme 1’ (2010) 436 pp., ISBN: 978-2-35158-106-3; e-ISBN: 978-2-35158-107-0; Ed. W. Brameshuber PRO 76: International Conference on ‘Material Science - HetMat - Modelling of Heterogeneous Materials - Theme 2’ (2010) 255 pp., ISBN: 978-2-35158-108-7; e-ISBN: 978-2-35158-109-4; Ed. W. Brameshuber PRO 77: International Conference on ‘Material Science - AdIPoC - Additions Improving Properties of Concrete - Theme 3’ (2010) 459 pp., ISBN: 978-2-35158-110-0; e-ISBN: 978-235158-111-7; Ed. W. Brameshuber PRO 78: 2nd Historic Mortars Conference and RILEM TC 203-RHM Final Workshop – HMC2010 (2010) 1416 pp., e-ISBN: 978-2-35158-112-4; Eds J. Válek, C. Groot, and J. J. Hughes PRO 79: International RILEM Conference on Advances in Construction Materials Through Science and Engineering (2011) 213 pp., e-ISBN: 978-2-35158-117-9; Eds Christopher Leung and K.T. Wan VI 5th Historic Mortars Conference – 19-21 June 2019 – Pamplona, Spain PRO 80: 2nd International RILEM Conference on Concrete Spalling due to Fire Exposure (2011) 453 pp., ISBN: 978-2-35158-118-6, e-ISBN: 978-2-35158-119-3; Eds E.A.B. Koenders and F. Dehn PRO 81: 2nd International RILEM Conference on Strain Hardening Cementitious Composites (SHCC2-Rio) (2011) 451 pp., ISBN: 978-2-35158-120-9, e-ISBN: 978-2-35158-121-6; Eds R.D. Toledo Filho, F.A. Silva, E.A.B. Koenders and E.M.R. Fairbairn PRO 82: 2nd International RILEM Conference on Progress of Recycling in the Built Environment (2011) 507 pp., e-ISBN: 978-2-35158-122-3; Eds V.M. John, E. Vazquez, S.C. Angulo and C. Ulsen PRO 83: 2nd International Conference on Microstructural-related Durability of Cementitious Composites (2012) 250 pp., ISBN: 978-2-35158-129-2; e-ISBN: 978-2-35158-123-0; Eds G. Ye, K. van Breugel, W. Sun and C. Miao PRO 85: RILEM-JCI International Workshop on Crack Control of Mass Concrete and Related issues concerning Early-Age of Concrete Structures – ConCrack 3 – Control of Cracking in Concrete Structures 3 (2012) 237 pp., ISBN: 978-2-35158-125-4; e-ISBN: 978-2-35158-126-1; Eds F. Toutlemonde and J.-M. Torrenti PRO 86: International Symposium on Life Cycle Assessment and Construction (2012) 414 pp., ISBN: 978-2-35158-127-8, e-ISBN: 978-2-35158-128-5; Eds A. Ventura and C. de la Roche PRO 87: UHPFRC 2013 – RILEM-fib-AFGC International Symposium on Ultra-High Performance Fibre-Reinforced Concrete (2013), ISBN: 978-2-35158-130-8, e-ISBN: 978-235158-131-5; Eds F. Toutlemonde PRO 88: 8th RILEM International Symposium on Fibre Reinforced Concrete (2012) 344 pp., ISBN: 978-2-35158-132-2, e-ISBN: 978-2-35158-133-9; Eds Joaquim A.O. Barros PRO 89: RILEM International workshop on performance-based specification and control of concrete durability (2014) 678 pp, ISBN: 978-2-35158-135-3, e-ISBN: 978-2-35158-136-0; Eds. D. Bjegović, H. Beushausen and M. Serdar PRO 90: 7th RILEM International Conference on Self-Compacting Concrete and of the 1st RILEM International Conference on Rheology and Processing of Construction Materials (2013) 396 pp, ISBN: 978-2-35158-137-7, e-ISBN: 978-2-35158-138-4; Eds. Nicolas Roussel and Hela Bessaies-Bey PRO 91: CONMOD 2014 - RILEM International Symposium on Concrete Modelling (2014), ISBN: 978-2-35158-139-1; e-ISBN: 978-2-35158-140-7; Eds. Kefei Li, Peiyu Yan and Rongwei Yang PRO 92: CAM 2014 - 2nd International Conference on advances in chemically-activated materials (2014) 392 pp., ISBN: 978-2-35158-141-4; e-ISBN: 978-2-35158-142-1; Eds. Caijun Shi and Xiadong Shen PRO 93: SCC 2014 - 3rd International Symposium on Design, Performance and Use of SelfConsolidating Concrete (2014) 438 pp., ISBN: 978-2-35158-143-8; e-ISBN: 978-2-35158-144-5; Eds. Caijun Shi, Zhihua Ou, Kamal H. Khayat PRO 94 (online version): HPFRCC-7 - 7th RILEM conference on High performance fiber reinforced cement composites (2015), e-ISBN: 978-2-35158-146-9; Eds. H.W. Reinhardt, G.J. Parra-Montesinos, H. Garrecht PRO 95: International RILEM Conference on Application of superabsorbent polymers and other new admixtures in concrete construction (2014), ISBN: 978-2-35158-147-6; e-ISBN: 978-235158-148-3; Eds. Viktor Mechtcherine, Christof Schroefl PRO 96 (online version): XIII DBMC: XIII International Conference on Durability of Building Materials and Components (2015), e-ISBN: 978-2-35158-149-0; Eds. M. Quattrone, V.M. John VII 5th Historic Mortars Conference – 19-21 June 2019 – Pamplona, Spain PRO 97: SHCC3 – 3rd International RILEM Conference on Strain Hardening Cementitious Composites (2014), ISBN: 978-2-35158-150-6; e-ISBN: 978-2-35158-151-3; Eds. E. Schlangen, M.G. Sierra Beltran, M. Lukovic, G. Ye PRO 98: FERRO-11 – 11th International Symposium on Ferrocement and 3rd ICTRC International Conference on Textile Reinforced Concrete (2015), ISBN: 978-2-35158-152-0; e-ISBN: 978-2-35158-153-7; Ed. W. Brameshuber PRO 99 (online version): ICBBM 2015 - 1st International Conference on Bio-Based Building Materials (2015), e-ISBN: 978-2-35158-154-4; Eds. S. Amziane, M. Sonebi PRO 100: SCC16 - RILEM Self-Consolidating Concrete Conference (2016), ISBN: 978-235158-156-8; e-ISBN: 978-2-35158-157-5 PRO 101 (online version): III Progress of Recycling in the Built Environment (2015), e-ISBN: 978-2-35158-158-2; Eds I. Martins, C. Ulsen and S. C. Angulo PRO 102 (online version): RILEM Conference on Microorganisms-Cementitious Materials Interactions (2016), e-ISBN: 978-2-35158-160-5; Eds. Alexandra Bertron, Henk Jonkers, Virginie Wiktor PRO 103 (online version): ACESC’16 - Advances in Civil Engineering and Sustainable Construction (2016), e-ISBN: 978-2-35158-161-2 PRO 104 (online version): SSCS'2015 - Numerical Modeling - Strategies for Sustainable Concrete Structures (2015), e-ISBN: 978-2-35158-162-9 PRO 105: 1st International Conference on UHPC Materials and Structures (2016), ISBN: 978-235158-164-3, e-ISBN: 978-2-35158-165-0 PRO 106: AFGC-ACI-fib-RILEM International Conference on Ultra-High-Performance FibreReinforced Concrete – UHPFRC 2017 (2017), ISBN: 978-2-35158-166-7, e-ISBN: 978-2-35158167-4; Eds. François Toutlemonde & Jacques Resplendino PRO 107 (online version): XIV DBMC – 14th International Conference on Durability of Building Materials and Components (2017), e-ISBN: 978-2-35158-159-9; Eds. Geert De Schutter, Nele De Belie, Arnold Janssens, Nathan Van Den Bossche PRO 108: MSSCE 2016 - Innovation of Teaching in Materials and Structures (2016), ISBN: 9782-35158-178-0, e-ISBN: 978-2-35158-179-7; Ed. Per Goltermann PRO 109 (2 volumes): MSSCE 2016 - Service Life of Cement-Based Materials and Structures (2016), ISBN Vol. 1: 978-2-35158-170-4, Vol. 2: 978-2-35158-171-4, Set Vol. 1&2: 978-235158-172-8, e-ISBN : 978-2-35158-173-5; Eds. Miguel Azenha, Ivan Gabrijel, Dirk Schlicke, Terje Kanstad and Ole Mejlhede Jensen PRO 110: MSSCE 2016 - Historical Masonry (2016), ISBN: 978-2-35158-178-0, e-ISBN: 978-235158-179-7; Eds. Inge Rörig-Dalgaard and Ioannis Ioannou PRO 111: MSSCE 2016 - Electrochemistry in Civil Engineering (2016), ISBN: 978-2-35158176-6, e-ISBN: 978-2-35158-177-3; Ed. Lisbeth M. Ottosen PRO 112: MSSCE 2016 - Moisture in Materials and Structures (2016), ISBN: 978-2-35158-1780, e-ISBN: 978-2-35158-179-7; Eds. Kurt Kielsgaard Hansen, Carsten Rode and Lars-Olof Nilsson PRO 113: MSSCE 2016 - Concrete with Supplementary Cementitious Materials (2016), ISBN: 978-2-35158-178-0, e-ISBN: 978-2-35158-179-7; Eds. Ole Mejlhede Jensen, Konstantin Kovler and Nele De Belie PRO 114: MSSCE 2016 - Frost Action in Concrete (2016), ISBN: 978-2-35158-182-7, e-ISBN: 978-2-35158-183-4; Eds. Marianne Tange Hasholt, Katja Fridh and R. Doug Hooton PRO 115: MSSCE 2016 - Fresh Concrete (2016), ISBN: 978-2-35158-184-1, e-ISBN: 978-235158-185-8; Eds. Lars N. Thrane, Claus Pade, Oldrich Svec and Nicolas Roussel VIII 5th Historic Mortars Conference – 19-21 June 2019 – Pamplona, Spain PRO 116: BEFIB 2016 – 9th RILEM International Symposium on Fiber Reinforced Concrete (2016), ISBN: 978-2-35158-187-2, e-ISBN: 978-2-35158-186-5; PRO 117: 3rd International RILEM Conference on Microstructure Related Durability of Cementitious Composites (2016), ISBN: 978-2-35158-188-9, e-ISBN: 978-2-35158-189-6; Eds. Changwen Miao, Wei Sun, Jiaping Liu, Huisu Chen, Guang Ye and Klaas van Breugel PRO 118 (4 volumes): International Conference on Advances in Construction Materials and Systems (2017), ISBN Set: 978-2-35158-190-2, Vol. 1: 978-2-35158-193-3, Vol. 2: 978-2-35158194-0, Vol. 3: ISBN:978-2-35158-195-7, Vol. 4: ISBN:978-2-35158-196-4, e-ISBN: 978-235158-191-9; Ed. Manu Santhanam PRO 119 (online version): ICBBM 2017 - Second International RILEM Conference on Bio-based Building Materials, (2017), e-ISBN: 978-2-35158-192-6; Ed. Sofiane Amziane PRO 120 (2 volumes): EAC-02 - 2nd International RILEM/COST Conference on Early Age Cracking and Serviceability in Cement-based Materials and Structures, (2017), Vol. 1: 978-235158-199-5, Vol. 2: 978-2-35158-200-8, Set: 978-2-35158-197-1, e-ISBN: 978-2-35158-198-8; Eds. Stéphanie Staquet and Dimitrios Aggelis PRO 121 (2 volumes): SynerCrete18: Interdisciplinary Approaches for Cement-based Materials and Structural Concrete: Synergizing Expertise and Bridging Scales of Space and Time, (2018), Set: 978-2-35158-202-2, Vol.1: 978-2-35158-211-4, Vol.2: 978-2-35158-212-1, e-ISBN: 978-235158-203-9; Ed. Miguel Azenha, Dirk Schlicke, Farid Benboudjema, Agnieszka Knoppik PRO 122: SCC’2018 China - Fourth International Symposium on Design, Performance and Use of Self-Consolidating Concrete, (2018), ISBN: 978-2-35158-204-6, e-ISBN: 978-2-35158-205-3 PRO 123: Final Conference of RILEM TC 253-MCI: Microorganisms-Cementitious Materials Interactions (2018), Set: 978-2-35158-207-7, Vol.1: 978-2-35158-209-1, Vol.2: 978-2-35158210-7, e-ISBN: 978-2-35158-206-0; Ed. Alexandra Bertron PRO 124 (online version): Fourth International Conference Progress of Recycling in the Built Environment (2018), e-ISBN: 978-2-35158-208-4; Eds. Isabel M. Martins, Carina Ulsen, Yury Villagran PRO 125 (online version): SLD4 - 4th International Conference on Service Life Design for Infrastructures (2018), e-ISBN: 978-2-35158-213-8; Eds. Guang Ye, Yong Yuan, Claudia Romero Rodriguez, Hongzhi Zhang, Branko Savija PRO 126: Workshop on Concrete Modelling and Material Behaviour in honor of Professor Klaas van Breugel (2018), ISBN: 978-2-35158-214-5, e-ISBN: 978-2-35158-215-2; Ed. Guang Ye PRO 127 (online version): CONMOD2018 - Symposium on Concrete Modelling (2018), eISBN: 978-2-35158-216-9; Eds. Erik Schlangen, Geert de Schutter, Branko Savija, Hongzhi Zhang, Claudia Romero Rodriguez PRO 128: SMSS2019 - International Conference on Sustainable Materials, Systems and Structures (2019), ISBN: 978-2-35158-217-6, e-ISBN: 978-2-35158-218-3; PRO 129: 2nd International Conference on UHPC Materials and Structures (UHPC2018-China), ISBN: 978-2-35158-219-0, e-ISBN: 978-2-35158-220-6; RILEM REPORTS (REP) Report 19: Considerations for Use in Managing the Aging of Nuclear Power Plant Concrete Structures (ISBN: 2-912143-07-1); Ed. D. J. Naus Report 20: Engineering and Transport Properties of the Interfacial Transition Zone in Cementitious Composites (ISBN: 2-912143-08-X); Eds. M. G. Alexander, G. Arliguie, G. Ballivy, A. Bentur and J. Marchand IX 5th Historic Mortars Conference – 19-21 June 2019 – Pamplona, Spain Report 21: Durability of Building Sealants (ISBN: 2-912143-12-8); Ed. A. T. Wolf Report 22: Sustainable Raw Materials - Construction and Demolition Waste (ISBN: 2-912143-17-9); Eds. C. F. Hendriks and H. S. Pietersen Report 23: Self-Compacting Concrete state-of-the-art report (ISBN: 2-912143-23-3); Eds. Å. Skarendahl and Ö. Petersson Report 24: Workability and Rheology of Fresh Concrete: Compendium of Tests (ISBN: 2-912143-32-2); Eds. P. J. M. Bartos, M. Sonebi and A. K. Tamimi Report 25: Early Age Cracking in Cementitious Systems (ISBN: 2-912143-33-0); Ed. A. Bentur Report 26: Towards Sustainable Roofing (Joint Committee CIB/RILEM) (CD 07) (e-ISBN 978-2-912143-65-5); Eds. Thomas W. Hutchinson and Keith Roberts Report 27: Condition Assessment of Roofs (Joint Committee CIB/RILEM) (CD 08) (e-ISBN 978-2-912143-66-2); Ed. CIB W 83/RILEM TC166-RMS Report 28: Final report of RILEM TC 167-COM ‘Characterisation of Old Mortars with Respect to Their Repair (ISBN: 978-2-912143-56-3); Eds. C. Groot, G. Ashall and J. Hughes Report 29: Pavement Performance Prediction and Evaluation (PPPE): Interlaboratory Tests (e-ISBN: 2-912143-68-3); Eds. M. Partl and H. Piber Report 30: Final Report of RILEM TC 198-URM ‘Use of Recycled Materials’ (ISBN: 2-91214382-9; e-ISBN: 2-912143-69-1); Eds. Ch. F. Hendriks, G. M. T. Janssen and E. Vázquez Report 31: Final Report of RILEM TC 185-ATC ‘Advanced testing of cement-based materials during setting and hardening’ (ISBN: 2-912143-81-0; e-ISBN: 2-912143-70-5); Eds. H. W. Reinhardt and C. U. Grosse Report 32: Probabilistic Assessment of Existing Structures. A JCSS publication (ISBN 2-912143-24-1); Ed. D. Diamantidis Report 33: State-of-the-Art Report of RILEM Technical Committee TC 184-IFE ‘Industrial Floors’ (ISBN 2-35158-006-0); Ed. P. Seidler Report 34: Report of RILEM Technical Committee TC 147-FMB ‘Fracture mechanics applications to anchorage and bond’ Tension of Reinforced Concrete Prisms – Round Robin Analysis and Tests on Bond (e-ISBN 2-912143-91-8); Eds. L. Elfgren and K. Noghabai Report 35: Final Report of RILEM Technical Committee TC 188-CSC ‘Casting of Self Compacting Concrete’ (ISBN 2-35158-001-X; e-ISBN: 2-912143-98-5); Eds. Å. Skarendahl and P. Billberg Report 36: State-of-the-Art Report of RILEM Technical Committee TC 201-TRC ‘Textile Reinforced Concrete’ (ISBN 2-912143-99-3); Ed. W. Brameshuber Report 37: State-of-the-Art Report of RILEM Technical Committee TC 192-ECM ‘Environmentconscious construction materials and systems’ (ISBN: 978-2-35158-053-0); Eds. N. Kashino, D. Van Gemert and K. Imamoto Report 38: State-of-the-Art Report of RILEM Technical Committee TC 205-DSC ‘Durability of Self-Compacting Concrete’ (ISBN: 978-2-35158-048-6); Eds. G. De Schutter and K. Audenaert Report 39: Final Report of RILEM Technical Committee TC 187-SOC ‘Experimental determination of the stress-crack opening curve for concrete in tension’ (ISBN 978-2-35158-0493); Ed. J. Planas Report 40: State-of-the-Art Report of RILEM Technical Committee TC 189-NEC ‘NonDestructive Evaluation of the Penetrability and Thickness of the Concrete Cover’ (ISBN 978-235158-054-7); Eds. R. Torrent and L. Fernández Luco Report 41: State-of-the-Art Report of RILEM Technical Committee TC 196-ICC ‘Internal Curing of Concrete’ (ISBN 978-2-35158-009-7); Eds. K. Kovler and O. M. Jensen X 5th Historic Mortars Conference – 19-21 June 2019 – Pamplona, Spain Report 42: ‘Acoustic Emission and Related Non-destructive Evaluation Techniques for Crack Detection and Damage Evaluation in Concrete’ - Final Report of RILEM Technical Committee 212-ACD (e-ISBN: 978-2-35158-100-1); Ed. M. Ohtsu Report 45: Repair Mortars for Historic Masonry - State-of-the-Art Report of RILEM Technical Committee TC 203-RHM (e-ISBN: 978-2-35158-163-6); Eds. Paul Maurenbrecher and Caspar Groot Report 46: Surface delamination of concrete industrial floors and other durability related aspects guide - Report of RILEM Technical Committee TC 268-SIF ( e-ISBN: 978-2-35158-201-5); Ed. Valérie Pollet XI 5th Historic Mortars Conference – 19-21 June 2019 – Pamplona, Spain Organizing Committee Conference Chair José Ignacio Álvarez (University of Navarra, Pamplona, Spain) Members (University of Navarra, Pamplona, Spain) José María Fernández Íñigo Navarro Adrián Durán Rafael Sirera Jesús Fidel González Burcu Taşcı Cristina Luzuriaga Joan Puig Max Renaud Petitjean Alessandro Speziale Scientific Committee Alvarez, José Ignacio. UNAV, Spain Maravelaki-Kalaitzaki, Pagona-Noni. TUC, Greece Biçer-Şimşir, Beril. GCI, USA Martínez Ramírez, Sagrario, IEM-CSIC, Spain Bokan Bosiljkov, Violeta. UL, Slovenia Pachta, Vasiliki. AUTh, Greece Faria, Paulina. NOVA de Lisboa, Portugal Papayianni, Ioanna. AUTh, Greece Groot, Caspar. UDelft, Netherlands Pavia, Sara. TCD, Ireland Gulotta, Davide. GCI, USA Hughes, John. UWS, U.K. Ioannou, Ioannis. UCY, Cyprus Rodríguez Navarro, Carlos. UGR, Spain Santos Silva, António. LNEC, Portugal Secco, Michele. UNIPD, Italy XIII Starinieri, Vincenzo. Sheffield Hallam University, U.K. Stefanidou, Maria. AUTh, Greece Theodoridou, Magdalini. Cardiff University, U.K. Valek, Jan. ASCR, Czech Republic Van Hees, Rob P.J. UDelft, Netherlands Veiga, Maria Rosário. LNEC, Portugal Velosa, Ana. University of Aveiro, Portugal 5th Historic Mortars Conference – 19-21 June 2019 – Pamplona, Spain Contents PREFACE............................................................................................................................................... 1 TOPIC 1: EARTH-BASED PLASTERS AND MORTARS ON ARCHAEOLOGY AND HISTORIC CONSTRUCTIONS .......................................................................................................... 3 Earth-based and current plasters: assessment of efficiency and contribution to indoor air quality .................. 5 Tânia Santos, Maria Idália Gomes, Flávia Coelho, Paulina Faria Earth-based plasters: the influence of clay mineralogy .................................................................................. 21 José Lima, Paulina Faria, António Santos Silva Rescuing the manufacturing process of traditional mortars present on XIX-century earthen buildings in Brazil .......................................................................................................................................................... 36 Andrea Cavicchioli, Isabela Ferreira Sodré dos Santos, João Guilherme Kimura Moreira, Lucy Gomes Sant'Anna Assessment of adhesive strength of an earth plaster on different substrates through different methods ..... 51 Paulina Faria, José Lima, João Nabais, Vitor Silva Similar appearance of mortar and brick masses in Algiers Casbah houses during the Ottoman period th th (16 - early 18 centuries) .............................................................................................................................. 65 Semha Bernou, Tsouria Kassab, Rosa Bustamante, Francisco Fernández Macroscopic high resolution techniques to the characterization the mortars structures in the Sé-Cathedral´s archaeological complex in Idanha-a-Velha (Portugal) ............................................................. 80 Pablo Guerra-García, Jorge Morín de Pablos, Isabel Sánchez Ramos TOPIC 2: USE OF NANOTECHNOLOGY FOR HIGH PERFORMANCE MORTARS ........... 93 Evaluation of the influence of nano-SiO2 and nano-Al2O3 on the physico-mechanical properties and microstructure of calcareous clay ................................................................................................................... 95 Eirini-Chrysanthi Tsardaka, Maria Stefanidou The use of nanoparticles to improve the performance of restoration mortars ............................................. 108 Beatriz Menéndez, Dita Frankeová, José Diaz, Radek Ševčík, Petra Macová, Mouna Faiz, Zuzana Slížková Evaluation of SiO2 nanoparticles as additive for lime mortars: changes in the microstructure and mechanical properties.................................................................................................................................. 121 María del Mar Barbero-Barrera, Aranzazu Sierra Fernández, Duygu Ergenc , Luz Stella Gomez Villalba, Rafael Fort Enhancing clay mortars’ properties .............................................................................................................. 132 A. Karozou, M. Stefanidou Study of the role of different nanoparticles in lime pastes ........................................................................... 144 Eirini-Chrysanthi Tsardaka, Maria Stefanidou Active photocatalytic-superhydrophobic coating with TiO2/ZnO nano-heterostructures for lime mortars... 155 Alessandro Speziale, Jesús Fidel González-Sánchez, Íñigo Navarro-Blasco, José M. Fernández, José I. Alvarez XIV 5th Historic Mortars Conference – 19-21 June 2019 – Pamplona, Spain TOPIC 3: GYPSUM-BASED PLASTERS AND MORTARS IN HISTORICAL CONSTRUCTIONS.......................................................................................................................... 169 Study of properties of gypsum plasters from Araripe’s Pole for application in restoration mortars ............. 171 Fernanda Cavalcanti Ferreira, Jose Getulio Gomes de Sousa, Arnaldo Manoel Pereira Carneiro Characterization of Gypsum Renders in the Paris Region and Determination of the Traditional Fabrication Process ...................................................................................................................................... 186 Jean Ducasse-Lapeyrusse, Véronique Vergès-Belmin The use of stucco-marble to restore veined polished limestone. The case of the pavement in the major sacristy of the Cathedral of Seville ............................................................................................................... 201 Antonio González Portillo, Maria Teresa Freire Stucco marble in the Portuguese architecture: first insights in mineralogical, physical and mechanical properties .................................................................................................................................................... 211 Maria Teresa Freire, António Santos Silva, Maria do Rosário Veiga Clay and gypsum mortars used during antiquity in Cyprus ........................................................................... 226 Maria Philokyprou Physical- mechanical comparison of the traditional gypsums from Albarracín and Pallars ........................... 237 David Osmar Batres Hernández, Antonia Navarro Ezquerra, Joan Ramon Rosell Amigó Detailed studies of gypsum plasters from the Ishrat Khana Mausoleum in Samarkand, Uzbekistan ............ 248 Steffen Laue TOPIC 4: FUNCTIONAL MORTARS FOR THE CONSERVATION OF HISTORIC AND MODERN CULTURAL HERITAGE STRUCTURES.................................................................. 259 Use of natural zeolite aggregate in restoration lime renders........................................................................ 261 Martin Vyšvařil, Patrik Bayer, Tomáš Žižlavský, Pavla Rovnaníková Fibre reinforced mortars for cultural heritage protection ............................................................................ 273 Miloš Drdácký, Dagmar Michoinová Comparative evaluation of the morphological and rheological characteristics of nanolime dispersions for the consolidation of architectural monuments................................................................................................... 283 Anastasia Michalopoulou, Elisavet Michailidi, Evangelos Favvas, Noni-Pagona Maravelaki, Vassilis Kilikoglou, Ioannis Karatasios Autogenic vs. autonomic self-healing process in conservation mortars with crystalline admixture ............. 296 Maria Amenta, Matina Papaioannou, Marios S. Katsiotis, Dimitris Gournis, Vassilis Kilikoglou, Ioannis Karatasios Addressing safety and durability requirements of architectural heritage by developing functional conservation mortars ................................................................................................................................... 307 Ioannis Karatasios, Zoi S. Metaxa, Stavros K. Kourkoulis, Nikolaos D. Alexopoulos, Vassilis Kilikoglou Self- healing lime-based mortars using biological mechanisms and microvascular networks ....................... 319 Cristina De Nardi, Magdalini Theodoridou, Philip Sim, Michael Harbottle, Anthoby D. Jefferson Hydrophobized lime grouts prepared with microsilica and superplasticizers ............................................... 330 Jesús Fidel González-Sánchez, Íñigo Navarro-Blasco, Adrián Duran, Rafael Sirera, José M. Fernández, José Ignacio Álvarez XV 5th Historic Mortars Conference – 19-21 June 2019 – Pamplona, Spain Photoactive Fe-TiO2 Lime Plasters for Building Protection ........................................................................... 346 Chrysi Kapridaki, Nikolaos Xynidis, Nikolaos Xekoukoulotakis, Nikolaos Kallithrakas-Kontos, Noni Maravelaki Lime-based rendering mortars with photocatalytic and hydrophobic agents: assessment of the water repellency and biocide effect ....................................................................................................................... 359 Jesús Fidel González-Sánchez, Burcu Taşcı, Guillermo Martínez de Tejada, José M. Fernández, Íñigo Navarro-Blasco, José Ignacio Alvarez SRG, Steel Reinforced Grout for strengthening masonry structures: from tests to applications ................... 373 Paolo Casadei, Paolo Girardello TOPIC 5: CHARACTERIZATION OF HISTORIC MORTARS AND MASONRY STRUCTURES. SAMPLING AND TEST METHODS ................................................................ 383 Calcite or quartz powder as aggregate of Roman plasters (Lombardy, Italy) ................................................ 385 Roberto Bugini, Luisa Folli Analytical and chromatic characterization of the interior walls finishes in the Batlló House of Gaudí in Barcelona. A surprising discovery ............................................................................................................. 396 Àgueda Serra, Joan Casadevall Roman mortars of floor substrates and walls from Arroyo de la Dehesa de Velasco site: petrographic and mineralogical characterization .............................................................................................................. 410 Ainhoa Alonso-Olazabal, Luis Ángel Ortega, Mª Cruz Zuluaga, Graciela Ponce, Javier Jiménez Echevarría, Carmen Alonso Fernández Provenance study of raw materials used for lime making at Prague Castle during medieval times .............. 424 Petr Kozlovcev, Jan Válek, Olga Skružná Interpretation of scientific data derived from analytical techniques used in the characterization of Roman mortars ........................................................................................................................................ 439 Duygu Ergenç, Rafael Fort, Nevin Aly, Olivier Henry, Sayed Hemeda Petrography of Historic Mortar Materials: Polarising Light Microscopy as a Method for Characterising Lime-Based Mortars ..................................................................................................................................... 453 Kristin Balksten, Bo Nitz, John J. Hughes, Jan-Erik Lindqvist Roman vs. medieval crushed brick lime mortars: A comparative study ........................................................ 468 Martin Schidlowski, Tobias Bader, Anja Diekamp A map is worth a thousand pictures: Using FTIR-imaging to analyze petrographic thin sections of historical and experimental mortar.......................................................................................................... 482 Anthony J. Baragona, Marta Anghelone, Johannes Weber Characterisation of concrete structures along the Reschen frontier, South Tyrol, Italy ................................ 495 Tobias Bader, Anja Diekamp Chemical, mineralogical and hydraulic characteristics of Roman mortars in Turkey..................................... 506 Burcu Taşcı, Hasan Böke ................................................................................................................................. 506 DB-HERITAGE: A database of mortars composition and characteristics........................................................ 516 António Santos Silva, Rodrigo Giollo, Maria João Correia, Maria do Rosário Veiga, Paulina Faria Algarve vernacular architecture facade ornaments: chemical and mineralogical characterization ............... 529 Marta Santos, António Santos Silva, Rosário Veiga XVI 5th Historic Mortars Conference – 19-21 June 2019 – Pamplona, Spain Characterisation methodology for lime based materials – A case study of the Rajagopuram of Pundarikaksha temple in Tamil Nadu, India ............................................................................................. 544 Divya Rani and Manu Santhanam Sampling cataloging methodology procedures for the conservation of historical colours in urban landscapes ..................................................................................................................................... 555 Isolina Díaz-Ramos, Jorge Manzano Cabrera Mineralogical characterization of historical cement-based mortars from Rupnik military fortification line ........................................................................................................................................... 565 Petra Štukovnik, Janez Peter Grom, Marjan Marinšek, Violeta Bokan Bosiljkov TOPIC 6: HISTORIC PRODUCTION, PROCESSING AND APPLICATION OF MORTARS, RENDERS AND GROUTS. LIME TECHNOLOGIES........................................... 577 Warm applied Mortar (WAM) – An insight into the historical technique of “Heiße Speis” and its use for renders ................................................................................................................................................... 579 Robert Wacha, Farkas Pintér Blast furnace slag in historic mortars of Bergslagen, Sweden ....................................................................... 585 Jan Erik Lindqvist, Kristin Balksten, Birgit Fredrich th Composition and Technology of the 17 Century Stucco Decorations at Červená Lhota Castle in the Southern Bohemia ............................................................................................................................. 596 Jan Válek, Olga Skružná, Petr Kozlovcev, Dita Frankeová, Petra Mácová, Alberto Viani, Ivana Kumpová Hot applied lime mortar – assessment of a traditional technique used in modern restoration .................... 614 Thomas Köberle, Matthias Zötzl, Alexander Fenzke, Heiner Siedel Preliminary research on potential raw material sources for dolomitic lime mortars at St. John’s convent at Müstair, Switzerland ................................................................................................... 628 Giovanni Cavallo, Marta Caroselli, Albert Jornet, Patrick Cassitti th th A Mortar Maker’s guide to evolving mortar specifications in 18 and 19 C France and England and their implications today ........................................................................................................................ 642 Lucie Fusade TOPIC 7: MORTARS IN ARCHAEOLOGICAL SITES. CONSTRUCTION HISTORY. ARCHAEOMETRY.......................................................................................................................... 653 Characterization and durability analysis of coral stones in a marine environment ....................................... 655 Swathy Manohar, Manu Santhanam Technical analysis on materials and characteristics of mortar-based compounds in Roman and Late antique Aquileia (Udine, Italy). A preliminary report of the results ............................................... 665 Simone Dilaria, Michele Secco, Jacopo Bonetto, Gilberto Artioli Fernandina old Wall of Lisbon – Characterization towards its preservation ................................................. 681 Leandro Gomes, Paulina Faria, Vitor Silva, António Santos Silva M.N.I.A.R. techniques of macroscopic characterization from the colorimetry and chromatographies analysis applied to the mortars in the archaeological site of Los Hitos (Arisgotas, Toledo, Spain) ................ 695 Pablo Guerra-García, Jorge Morín de Pablos, Isabel Sánchez Ramos XVII 5th Historic Mortars Conference – 19-21 June 2019 – Pamplona, Spain Analysis of mortar samples from the Church of the Saints Sergius and Bacchus at Umm as-Surab (Jordan) ................................................................................................................................ 713 Piero Gilento, Cecilia Pesce, Giovanni Pesce Characterisation of Roman Mortar from the Archaeological Site of Mirobriga ............................................ 727 Alvin Sern Hao Chua, Cristina Galacho, Patrícia Moita, José Carlos Quaresma Insights into Carolingian construction techniques – results from archaeological and mineralogical studies at Müstair Monastery, Grisons, Switzerland .................................................................................... 743 Marta Caroselli, Christine Bläuer, Patrick Cassitti, Giovanni Cavallo, Irka Hajdas, Sophie Hueglin, Hans Neukom, Albert Jornet Animal, Vegetable or Mineral? Characterising shell-lime, maerl-lime and limestone-lime mortar evidence from the Late Norse and Medieval site of Tuquoy, Orkney ........................................................... 758 Mark Thacker, John Hughes, Nic Odling TOPIC 8: DATING OF HISTORIC MORTARS.......................................................................... 779 An Ecology of Castle Construction: geoarchaeology, archaeobotany & radiocarbon analysis in the ecotone of Lochindorb Castle ............................................................................................................. 781 Mark Thacker Characterization of historic mortars: techniques used to establish a construction chronology. Case study: “Aragoneses’ Mill” as it belongs to popular architectural heritage ............................................ 800 Esther Moreno Fernández, Javier Pinilla Melo, Francisco González Yunta, Alberto Sepulcre Aguilar, Ignacio Lombillo Vozmediano, Yosbel Boffill Orama TOPIC 9: NATURAL AND ROMAN CEMENT MORTARS ..................................................... 817 From marlstone to rotary kilns – the early development of Portland cements in Central Europe ................ 819 Farkas Pintér, Christophe Gosselin, Thomas Köberle, István Vidovszky, Johannes Weber European natural cements - their key technical properties under standardised conditions ......................... 833 David Hughes, Johannes Weber, Vincenzo Starinieri, Farkas Pinter, Christophe Gosselin, Steven Feldman, Cecilia Pesce Restoration techniques using 1930’s Portland cements at Porte de l’Est in the Roman city-wall of Aventicum, Switzerland ........................................................................................................................... 848 Christophe Gosselin, Noé Terrapon Drying Shrinkage of Historic Portland Cements: Factors to be Considered for Successful Repair .................. 862 Simeon Wilkie, Thomas Dyer Repairs to Historic Concrete Pavement at Jacob Riis Park Utilizing Natural, Roman and Portland Cements ........................................................................................................................................ 877 Michael P. Edison Methodology of identification of natural and historic Portland cements. Application and study in mortars of Madrid and Barcelona............................................................................................................. 886 Cristina Mayo Corrochano, Judith Ramírez-Casas, David Sanz Arauz, Antonia Navarro Ezquerra, Juan Ramon Rosell Amigo The use of mortars in Palau Güell by Antoni Gaudi ...................................................................................... 901 Ricardo Gomez-Val, Judith Ramirez-Casas, Antonia Navarro-Ezquerra XVIII 5th Historic Mortars Conference – 19-21 June 2019 – Pamplona, Spain When Portland cement meets natural cement............................................................................................. 914 Elisabeth Marie-Victoire, Myriam Bouichou TOPIC 10: CONSERVATION ISSUES CONCERNING MORTARS, PLASTERS, RENDERS AND GROUTS. DIAGNOSIS. DECAY AND DAMAGE MECHANISMS. CASE STUDIES................................................................................................................................ 929 th Decorative renders simulating stone of middle 20 century in the region of Lisbon .................................... 931 Maria do Rosário Veiga, António Santos Silva, Cláudia Martinho, Paulina Faria The analysis of the proportion of mortar for Japanese roof tile (Ibushikawara) in Taiwan by applying of Taguchi Method ....................................................................................................................................... 944 Mei-Tsu Hsu, Bing-Sheng Yu th Evolution of mortars composition and characteristics during the 20 century– Study of Portuguese buildings awarded with Architecture Valmor Prize ...................................................................................... 959 Luís Almeida, António Santos Silva, José Mirão, Maria do Rosário Veiga Practical application of lime-pozzolan mortars to damp masonry ................................................................ 973 Dita Frankeová, Dana Janotová, Zuzana Slížková th The use of dolomitic lime in mortar samples from a 15 -century buttress of York Minster (York, UK) ........ 986 Cecilia Pesce, Alick Leslie, Alison Henry, John David, Giovanni Pesce The Restoration of the church of Our Lady of the Assumption, Dauis, Bohol, Philippines ............................ 997 Jim Franklin O. Kalaw, Raul Y. Naguit Jr Digital image analysis as basis for the evaluation of repair mortars in architectural conservation ............. 1008 C. Kaiser, L. Oetinger, R. Killian TOPIC 11: PRESERVATION. CONSOLIDATION MATERIALS AND TECHNIQUES. DEVELOPMENT OF NEW PRODUCTS. PREVENTIVE CONSERVATION ..................... 1021 Frost resistance of reproduced mosaic mortars ......................................................................................... 1023 Pavla Bauerová, Pavel Reiterman, Eva Vejmelková, Martin Keppert Preliminary results on the use of ammonium phosphate solutions for the consolidation of lime-based mortars ...................................................................................................................................................... 1032 Enrico Sassoni, Cesare Pizzigatti, Elisa Franzoni Comparative study of ethyl silicate versus acrylic resin consolidation of wall painting with high water and salts contents: a case study at the Chapter Hall of Chartres cathedral ............................... 1040 Laura Normand, Stéphanie Duchêne, Véronique Vergès-Belmin, Claire Dandrel, David Giovannacci, Witold Nowik Comparative analysis of permeability values of traditional aerial lime mortars for preventive conservation ............................................................................................................................ 1056 Ana González-Serrano, Reyes Rodríguez-García, Esther Ontiveros-Ortega Challenges and strategies of preventive conservation in places of worship – Church of Nossa Senhora de Guadalupe case study ............................................................................................... 1068 Alexandra Marco, Manuela Pintado, Patrícia R. Moreira, Eduarda Vieira XIX 5th Historic Mortars Conference – 19-21 June 2019 – Pamplona, Spain TOPIC 12: REPAIR MORTARS AND GROUTS. REQUIREMENTS AND DESIGN. COMPATIBILITY ISSUES. DURABILITY AND EFFECTIVENESS. REPAIR MORTARS: ADEQUACY OF TESTING PROCEDURES ....................................................... 1085 Effects of natural zeolite addition to lime based render layers for restoration of historical buildings ........ 1087 Marina Aškrabić, Dimitrije Zakić, Aleksandar Savić, Ljiljana Miličić Use of ultrafine mafic rocks for the enhancement of carbonation reaction in lime renders ....................... 1099 Loucas Kyriakou, Ioannis Rigopoulos, Ioannis Ioannou Microstructure of lime pastes with the addition of vegetable oils ............................................................. 1112 Cristiana Nunes, Alberto Viani, Kateřina Mlsnová, Dita Frankeová, Petra Mácová Improvements to Water, Salt-Scaling and Freeze-Thaw Resistances of Historic Mortar Replication Mixes ....................................................................................................................................... 1125 Michael P. Edison, Chad Lausberg Formulated lime mortars as a sustainable practice for Built Heritage conservation in Mexico ................... 1142 Marlene Sámano Chong The impact of elevated temperatures on the properties of lime-based mortars ........................................ 1156 Vasiliki Pachta, Sofia Triantafyllaki, Maria Stefanidou Characterization and compatibility assessment of commercial stone repair mortars ................................. 1166 Barbara Lubelli, Timo G. Nijland, Rob P.J. van Hees Impact of aggregates on fresh mortars’ properties .................................................................................... 1180 Ana Rita Santos, Maria do Rosário Veiga, António Santos Silva, Jorge de Brito NHL-based plasters and renders – Assessing the influence of mixing method on workability and hardened mortar properties ................................................................................................................ 1195 Frowin Ruegenberg, Martin Schidlowski, Tobias Bader, Anja Diekamp Lime-based grouts for architectural surface repair. Comparison of their performance by using laboratory and field test methods .............................................................................................................. 1215 Vasiliki Pachta, Ioanna Papayianni, Thomas Spyriliotis Evaluation of the fresh state properties of lime-based grouts through inter-laboratory comparative testing ................................................................................................................................... 1225 Vasiliki Pachta, Davide Gulotta, Jan Valek, Ioanna Papayianni Lime-pozzolan injection grouts with ovalbumin and ethanol added as water-reducing agents: grout design and assessment of the mineralogical evolution ..................................................................... 1238 Chiara Pasian, Michele Secco, Francesca Piqué, Gilberto Artioli, Sharon Cather Limestone-filled, hydraulic-lime mortars for historic and traditional fabrics .............................................. 1251 Marwa Aly, Sara Pavía Comparing the moisture permeability of limecrete and concrete floor slabs ............................................. 1267 Grace A. Phillips, Kevin Briggs, Iain McCaig, Richard J. Ball Impact of guar gum and chitosan ethers on physico-mechanical properties and durability of natural hydraulic lime mortars ............................................................................................................... 1279 Tomáš Žižlavský, Martin Vyšvařil, Patrik Bayer, Pavla Rovnaníková XX 5th Historic Mortars Conference – 19-21 June 2019 – Pamplona, Spain Technical analysis on materials and characteristics of mortar-based compounds in Roman and Late antique Aquileia (Udine, Italy). A preliminary report of the results Simone Dilaria1, Michele Secco2, Jacopo Bonetto3, Gilberto Artioli4 (1) University of Padova, Department of Cutural Heritage, simone.dilaria@phd.unipd.it (2) University of Padova, Department of Civil, Environmental and Architectural Engineering (ICEA); Interdepartmental Research Center for the Study of Cement Materials and Hydraulic Binders (CIRCe), michele.secco@unipd.it (3) University of Padova, Department of Cutural Heritage, jacopo.bonetto@unipd.it (4) University of Padova, Inter-departmental Research Center for the Study of Cement Materials and Hydraulic Binders (CIRCe); Department of Geosciences, University of Padova, Italy, gilberto.artioli@unipd.it Abstract In the present paper we report the preliminary results of an ongoing research focused on the investigation of Roman mortars and concretes employed in Aquileia from Roman to Early Medieval Age (II century BC – VI century AD). More than 250 samples have been collected from buildings spread all over of the town, with different chronologies of construction and different functions. Material characterization was achieved throughout a multi-analytical approach comprising optical microscopy (OM), X-Ray powder diffraction (XRPD) and Scanning Electron Microscopy-Energy Dispersive microanalysis (SEM-EDS). Analytical data have been strictly crosschecked in relation with the chronology and purpose of the structure from which mortars have been collected from. The preliminary results we obtained are providing intriguing outcomes: we observed a high specialization on “recipes” in relation to the function of mortars and concretes, but also chronology of production appears to have an important role in the composition of mortar-based compounds. Such an extensive sampling is giving valuable insights to decipher the relations among crafts and artisans in ancient construction and decorative activities. Introduction and state of art The present project is part of a larger research promoted by the Department of Cultural Heritage and the Department of Geosciences of the University of Padova, aimed at the investigation of types and characteristics of mortars and concretes exploited in ancient times. In the wake of the recent impulse devoted on studies concerning the “Archaeology of Architecture”, “Archaeology of Construction” and “Archaeology of building materials”, the ancient Provincia Cisalpina, corresponding to the actual northern Italy, has become, in the last decades, a fertile territory for archaeological and archaeometric researches. The results of these studies are demonstrating how Roman architecture in Cisalpina deeply differs from centre-southern Italian constructive traditions, in terms of forms, materials and techniques employed by ancient crafts [1-3]. 665 5th Historic Mortars Conference – 19-21 June 2019 – Pamplona, Spain Nevertheless, specific analytical researches on mortar-based materials have not been carried out in such a way as it has been done for centre-southern Italy, where the cases of Rome and Pompeii remain emblematic terms of comparison for these definite topics [4]. On the other hand, an analytical approach for the study of mortars and concretes has been rarely undertaken for significant case studies in the Roman Cisalpina. Wall-paintings are surely the materials on which mayor part of the researches have been based on, even if a main focus was dedicated to the characterization of pictorial layers, more than the analysis of supporting mortars (tectorium). Lombardy [5], North-Eastern Italy [6, 7, 8] and, in the last years, Slovenia (Emona-Ljubljana) [9] are the regions on which the sampling has been carried out in a more exhaustive way in statistical terms, as, since the ’90, more than 200 wallpaintings have been taken into exam. On the other hand, no extensive analytical datasets are available for other typologies of mortar-based compounds. Exceptions are represented by analyses on a targeted sampling of structural mortars employed in specific contexts such as Padova [10], Ravenna [11], Desenzano (Brescia) [12], Milan [13], Susa, the ancient Segusium (Turin) [14, 15] and Mošnje (Slovenia) [16]. Finally, other types of mortar-based materials employed in antiquity, for instance the ones manufactured for flooring purposes, have been traditionally investigated in relation to restoration activities. Specific studies on mortar bedding screeds have been performed on Roman pavements of Montegrotto (Padua) [17] and Cremona [18]. In this scenario, Aquileia represents a perfect context for developing a research on mortarsbased compounds which were, in the last years, only marginally investigated [1, 19]. During Roman times, Aquileia was one of the most prosperous towns of the Northern Italy and an important centre for the development of trends and practices in the field of art and architecture. After being established in 181 BC, the city become, during the Imperial age, a flourishing urban centre, as it was enriched by monumental buildings and highly prestigious private residences. In the IV century AD, it was considered by Ausonius (XI, 9, 4) one of the nine most important and extended cities of the ancient world, but in the 425 AD Aquileia collapsed under Attila’s invasion and the town was progressively abandoned by the end of the V century [20]. All these different historical periods are represented by the buildings that modified the shape and the plan of the city. In the last decade new impulse on excavations activities was promoted thanks to the contribution of Universities and private foundations such as Fondazione Aquileia, leading excavation, valorisation and preservation projects in several archaeological areas of the ancient town. Along with archaeological excavations and restoration activities, the University of Padova promoted research projects focused on the analysis on building techniques [3], mosaic art [21] and pictorial culture [22] in Aquileia. 666 5th Historic Mortars Conference – 19-21 June 2019 – Pamplona, Spain In the wake of this solid historic-archaeological background, these researches have established a fertile ground to fully immerge and contextualize the results of an analytical project focused on mortars-based materials characterization 4. Preliminary publications on this topic have revealed the potentialities of the exploitation of the single context approach in order to acquire a full and deep knowledge on characteristics of mortars and concretes employed along space and time in a determined area [23, 24, 25, 26, 27, 28]. The data in course of acquisition are providing new lymph for a thorough discussion on the issues related to competences and know-how of ancient crafts and artisans, their correlation with economic power of patronage, function of buildings and chronology of construction, in the framework of a realistic reconstruction of the history and economy of an ancient Roman town. Investigation contexts and sampling In order to crosscheck the characteristics of mortar-based materials employed in archaeological complexes with different chronology, social level and functional destination (i.e. private contexts, public buildings, defensive systems, suburban quarters etc.), a series of archaeological areas of the ancient city of Aquileia have been taken into exam (Figure 1). Main contexts are represented by houses (Domus of Tito Macro, Domus of Bestie Ferite [29], Domus at Stalla Violin [30]) which life spans from the I century BC to the V century AD, along with periodic renovations activities that determined frequent reconstruction of floors, canalizations and wall structures; public buildings are represented by the theatre [31] and the amphitheatre [32], that were probably established during the early imperial age, and by the mayor Roman thermal complex of the city, the so-called Thermae Felices Constantinianae, which were probably built under the patronage of the Constantine family during the IV century AD [33]; defensive architecture has been considered, as the city walls were taken into exam along with their construction phases, ranging from the period of foundation of the city throughout reconstructions and modifications during Late Antiquity and Byzantine age [34]; Aquileia suburb was also examined by investigating of structures in a productive area in the immediate surrounding of the city [35]. More than 200 samples of mortars and concretes have been collected from the cited sites. Samples refer to a) foundations mortars (sometimes acquired by the direct sampling of core drillings); b) wall jointing mortars and wall core mortars; c) concrete vaults; d) floors and floor beddings (mosaic, concrete floors, brick floors, opus sectile floors, mortar floors); e) structural and revetment mortars of hydraulic systems (water tank, canalization conducts, 4 The current research has been supported by the Superintendence of Archaeology, Fine Arts and Landscape of Friuli Venezia Giulia and by research teams of the Universities currently involved in the annual archaeological excavations in the ancient city. In particular, we are grateful for the collaboration of the excavation directors of the investigated sites in Aquileia: Prof. J. Bonetto and Prof. M. Salvadori (Dep. of Cultural Heritage, University of Padova); prof. P. Basso (Dep. of Culture and Civilization, University of Verona); prof. D. Cottica (Dep. of Humanities, University Ca' Foscari of Venice); prof. M. Rubinich (Department of Humanistic Studies and Cultural Heritage, University of Udine). 667 5th Historic Mortars Conference – 19-21 June 2019 – Pamplona, Spain piscinae) 5. Apart from the mortar samples taken directly on site, more than 60 wall-painting fragments have been also analysed, mainly collected from the materials conserved in the deposits of the Archaeological Museum of Aquileia and usually recovered during excavations conducted in last century in different areas of Aquileia. Samples were taken from assemblages of well dated wall painting fragments which were already studied according to stylistic features [25, 28]. Figure 1. Aquileia. Plan of the investigated archaeological sites. a) mosaic bedding screed at Domus of Bestie ferite; b) collapsed vault of Thermae Felices Constantinianae; c) core drilling in theatre foundation platform; d) jointing mortars of the amphiteatre; e) wall of eastern fluvial bank; f) joint mortar with shell aggregates of Bizantine city walls. Methodology The collected samples have been analysed following a multi analytical approach. Firstly, all the samples have been described according to their macroscopic features (Figure 2). A preliminary petrographic study through optical microscopy (OM) was then performed on all the analysed samples following macroscopic and microstratigraphic procedures for mortarbased materials described in UNI Norm 11176:2006 “Cultural heritage - Petrographic description of a mortar”. The study was performed both by optical microscopy (OM) on 30 μm thin sections, obtained by vacuum impregnating portions of the materials with epoxy resin and sectioning them transversally (Figure 3). Mineralogical quantitative phase analyses (QPA) were performed on a selection of representative samples through X-ray powder diffraction (XRPD). Then, QPA’s were performed using the Rietveld method [36]. XRPD analyses on the sole binder fraction were performed after separation through the Cryo2Sonic 2.0 procedure [37] in order to 5 Mortar-based compounds from hydraulic structures are still under examination and they will be not discussed in the present paper. 668 5th Historic Mortars Conference – 19-21 June 2019 – Pamplona, Spain properly define hydraulic phases on those samples showing pozzolanic properties after OM or XRPD bulk examinations. The determination of both crystalline and amorphous content was calculated by adding 20% wt. of ZnO to the powders as internal standard. Figure 2. Macroscopic images of mortar-based compounds. a) sample from the theatre opus caementicium substructure (cross section); b) sample from the amphitheatre opus caementicium substructure (cross section after consolidation in epoxy resin); c) wall joint mortar from Domus of Tito Macro (cross section); d) wall joint mortar from Domus of Tito Macro (petrographic section after consolidation in epoxy resin); e) late antique floor bedding from Domus of Bestie Ferite (petrographic section); f) concrete vault from Thermae Felices Constantinianae; g) IInd style wall painting from Domus of Bestie Ferite (cross section); IVth cen. AD wall painting from Teodorian complex (cross section). 669 5th Historic Mortars Conference – 19-21 June 2019 – Pamplona, Spain Figure 3. Petrographic analysis on thin section of mortar-based compounds. a) OM-TL-Pn, theatre mortar from platform foundational opus caementicium (Cg: carbonate gravel); b) OM-TL-Xn, terracotta dust (Td) and terracotta fragments (Tf) with secondary aliquots of carbonate sand (Cs) from the bottom cocciopesto layer of theatre platform foundation; c) OM-TL-Xn, square rubble masonry wall joint mortar (Cg: carbonate gravel; Ch: chert); d) OM-TL-Xn, brick wall joint mortar (Lp: lime lump); e) OM-TL-Xn, pyroxenes (Px) and volcanic (Vc) aggregates in a wall joint mortar, with subordinated feldspars (Fs) and quartz (Qz); f) OM-TL-Xn, Late Antique wall joint mortar with diffuse presence of lime lumps (Lp); g) cross section of I cen. AD mosaic bedding screed (Lt: limestone tesserae; Pl: lime-putty setting bed; Tf: terracotta fragments of the nucleus; h) OM-TL-Pn, Ist style wall painting, intonachino layer with diffuse euhedral spathic calcite. (OM: optical microscopy; TL: transmitted light; Xn: crossed nicols; Pn: parallel nicols) Data were collected using a Bragg–Brentano θ–θ diffractometer (PANalytical X’Pert PRO, Co– Kα radiation, 40kV and 40 mA) equipped with a real-time multiple strip (RTMS) detector 670 5th Historic Mortars Conference – 19-21 June 2019 – Pamplona, Spain (X’Celerator by Panalytical). Divergence and anti-scattering slits, of 0.5° and 1° respectively, were mounted in the incident beam pathway. The pathway of the diffracted beam included a Ni filter, a Soller slit (0.04 rad) and an antiscatter blade (5 mm). Data acquisition was performed by operating a continuous scan in the range 3–80° 2θ, with a virtual step scan of 0.02° 2θ. Diffraction patterns were interpreted using the X’Pert HighScore Plus 3.0 software by PANalytical, qualitatively reconstructing mineral profiles of the compounds by comparison with PDF databases from the International Centre for Diffraction Data (ICDD). Then, QPAs were performed using the Rietveld method. Refinements were accomplished using the TOPAS software (version 4.1) by Bruker AXS. Finally, the thin section samples were microstructurally and micro chemically characterized by Scanning Electron Microscopy (SEM). A CamScan MX2500 scanning electron microscope was used, equipped with a LaB6 cathode and a four-quadrant solid state BSE detector for imaging. The analytical conditions were as follows: accelerating voltage 20 kV; filament current 1.80 A; emission current 20 μA; aperture current 300 nA; working distance 20–30 mm. Furthermore, an EDAX–EDS energydispersive X-ray fluorescence spectrometer was used for chemical microanalysis, mounted with a Sapphire Detector composed of a LEAP+ Si(Li) crystal and a Super Ultra Thin Window. Preliminary results Even if the investigations on mortar-based samples are still ongoing, some preliminary results can be here outlined. The results showed high variability on mortar and concrete “recipes”, depending on their function in structures and chronology of production. Foundations Foundational mortars are mainly represented by samples collected from core drillings performed in the substructures of the theatre and amphitheatre of Aquileia, from the upper portion of ground platform of the Thermae Felices Constantinianae, and from a particular opus caemeticium [38] foundation casting identified at the basis of the south-eastern part of the Republican city walls. Different “recipes” were employed in these structures. In both the theatre and amphitheatre platforms, the foundations were made with a > 3 m deep opus caementicium structure made of a mixture of lime, gravel and sand to which decimetre sized limestone fragments were added [38]. Petrographically (Figure 2, a-b; Figure 3, a), aggregate fraction is represented by carbonates and secondary silicates (chert, quartz) compatible with sands and gravels locally sourced from river bed deposits of Natiso/Torre and Isonzo [39]. SEM-EDS analysis clearly detected de-dolomitization of dolostone aggregates (Figure 4, a) and alkali-silica reactions of chert (Figure 4, b-c) in the mortars of the opus caementicium foundation of the theatre of Aquileia, which produced a diffuse silicate-magnesian gel in the matrix, deeply permeated with calcium of binder fraction [40]. Being absent pozzolanae of fictile fraction, it is possible that the use of salt water in the preparation of the mixture could have determined a highly alkaline pH in the compounds activating de-dolomitization and silica reaction of chert fragments [41]. Crystalline C-S-H of AFm phases have not been 671 5th Historic Mortars Conference – 19-21 June 2019 – Pamplona, Spain detected after XRPD bulk analysis. At the base of the theatre foundation platform a layer of fine cocciopesto [38] was placed, probably to contrast rising ground water enhancing waterproofing properties and avoiding water infills (Figure 3, b). Figure 4. SEM-EDS of theatre opus caementicium foundations (BSE images). a) dolostone clasts with clear dedolomitization phenomena; a1) EDS microanalysis of an un-altered dolostone relict; a2) EDS analysis of dedolomitized dolostone interface with binder matrix; a3) EDS analysis of mortar matrix; a4) EDS microanalysis of nodules of pure carbonates in mortar matrix; b) altered chert fragments; c) highlighted area of the figure b; c1) EDS analysis of an highly altered portion of a chert fragment with Ca/Mg ions permeated from the matrix; c2) EDS analysis of a chert relict feebly altered. Figure 5. XRPD patterns of the binder fractions of selected hydraulic mortars, with highlighted the main diffraction peaks of the anthropogenic binding phases: a) theatre, cocciopesto mortar at the base of the foundation platform; b) Thermae Felices Constantinianae, coating mortar of a pool; c) Republican city walls, foundational concrete. 672 5th Historic Mortars Conference – 19-21 June 2019 – Pamplona, Spain OM coupled with XRPD binder analyses demonstrated the presence of diffused terracotta dust in the foundational cocciopesto layer of the theatre, which determined the formation of moderate AFm hydrated phases (Figure 5, a). Cocciopesto mortars with significant amounts of fine terracotta dust have been employed also in the foundations and several other structures of the Thermae Felices Constantinianae. Also in this case, XRPD binder fraction analyses showed the formation of AFm hydrates, indicating the occurrence of pozzolanic reaction processes (Figure 5, b). From a petrographic point of view, also the opus caemetitium structures in the foundations of Republican walls seem to be realized with the traditional mix of raw material defined above in relation to the theatre and amphitheatre foundations. However, the high strength and cohesion of this compound is an indication of relevant hydraulic reaction, as confirmed by the occurrence of Tobermorite 14A and AFm hydraulic phases in the binder fractions (Figure 5, c). The formation of hydrated phases appears to be due to the presence in the matrix of high silica aliquots responsible for the diffuse formation of pure C-S-H. Being absent clasts of volcanoclastic pozzolanae (as previously supposed [24]) or dusty terracotta fraction, it is probable that a cherty limestone could have been calcined in order to obtain a natural hydraulic lime, as supposed also in the case of the Ponte di Augusto in Narni [42]. Chert aggregate fraction added to the mortars could have been another secondary activator of the pozzolanic reaction [43], mainly if combined with salt water, as previously observed in relation with the theatre. Wall structures During the Republican and Proto-Imperial ages, walls in Aquileia were usually made with limestone or sandstone coursed square rubble masonry [3]. Jointing mortars were produced with lime mortars. The aggregate fraction is represented by dominant carbonate lithic particles, with secondary aliquots of chert and quartz and traces of sandstones, with binder/aggregate (B/A) ratios around 1:2 (Figure 2, c; Figure 3, c). In the case of brick walls [3], finer mortars produced mixing lime and well-graded carbonate/silicate sand were most commonly employed (Figure 2, d; Figure 3, d). Mineralogical analyses on bulk samples revealed calcite and dolomite as prevalent fraction, while feldspars and micas occur in modest amounts always < 5%. Amorphous and smectite phases are related mainly to clay inclusions which are present, in different aliquots, in all the compounds. Also in this case, in mayor part of the samples aggregate sands and gravels are locally sourced from river bed deposits of Natiso/Torre and Isonzo [39]. Only in a few occasion aggregates are not local. This is the case of two jointing mortar samples were aggregates are represented by abundant pyroxenes, volcanic clasts and feldspars (Figure 3, e). It is possible to assume that these non-local sands represent the reuse of ballast bags which originally reached Aquileia via fluvial or terrestrial routes. 673 5th Historic Mortars Conference – 19-21 June 2019 – Pamplona, Spain In other occasions, mortars with high ratios of chert gravels were used in the walls of the Republican Domus of Tito Macro. The high oxidization of chert and carbonate aggregates, as well as the absence of dolomite fraction, indicate a possible provenance from paleo fluvial deposits, partially pedogenized, which should be located in the fluvial plain of the foothills area of Friuli region, northern of Aquileia 6. The reason for the choice of these quarrying basins is still unclear. It has been observed a progressive modification in “recipes” of jointing wall mortars, as revealed from the analysis of IV-V century AD city wall and housing structures. Late Antique mortar-based compounds present high lime binder fraction in B/A ratios of ≥ 1:1, highly sorted carbonate aggregates and frequent lime lumps inclusions (Figure 3, f). The widespread praxis of spoliation and calcination of limestones and marbles during late antiquity, observed also in the case of Aquileia [3], could be addressed as a cause of the large availability of quicklime that could have determined this variation of “recipes”. Finally, it has been observed the use of shells as aggregate fraction in the mortars of the Bizantine city defensive system. This characteristic appears to be common in Bizantine period: shell-rich mortars have been employed in the jointing mortars of city walls of Leptis Magna, but attestation of these practices traces back even to the Minoan period [44]. The presence of prevalent coastal shell species, probably coming from beach shoreline proximal area, demonstrates the substantial modification of sand quarry zones, probably as consequence of the loss of control of the inland territories north of Aquileia after barbarian invasions [20]. Vaults Three samples of mortars from the vaults of the Late Antique Thermae Felices Constantinianae have been analysed. As widely documented in literature [45], lightweight caementa were employed as aggregate in order to reduce the weight of the vaults of Thermae Felices Constantinianae. In this context, lightweight ceamenta are constituted of three different species of vulcanic tuff scoria which were surely imported (Figure 2, f), considering that there are no such formations in the Friulan territories and surrounding areas. Petro-chemical trace elements analyses will be performed for the determination of the provenance of these materials. The results will be compared with the volcanoclastic tuff and scoria petrochemical signature database of the Latial and Campanian volcanic formations [46, 47]. Floors and floor beddings Floor bedding mortars refer mainly to mosaics and opus sectile bedding screeds. As recently published [23, 26], we observed that Late Republican and Proto-Imperial mosaic were realized over bedding screeds generally composed of two layers. The inner one, that can be 6 We are grateful for the advice to prof. A. Fontana, University of Padova. 674 5th Historic Mortars Conference – 19-21 June 2019 – Pamplona, Spain associate with the Vitruvian rudus (VII, 1, 3), is made of a concrete with broken terracotta fragments composed of sole lime and centimeter sized terracotta fragments [38]; the outer layer, that can be associated with the nucleus (VII, 1, 3), is a cocciopesto mortar made of lime and millimeter-sized terracotta fragments [38]. In high-quality mosaics, tesserae were usually placed over a millimeter-thick layer of pure lime-putty [38] sometimes mixed with sparse spathic calcite (Figure 3, g). Even if not attested in ancient literature, this stratum has been already observed [48] and it was probably made to allow a more precise setting of the tesserae along during the mosaic production. Opus sectile pavements were placed over thicker screeds made of cocciopesto mortars or concrete with broken terracotta. The presence of diffuse terracotta dust, observed via OM analyses, substantially distinguish mortar-based compound for opus sectile screeds from the mosaic bedding ones. Also in this case, a variation along time of materials and “recipes” has been proved. If opus sectile construction traditions do not seem to be substantially modified along time, Late Antique mosaics bedding mortars in private contexts (houses) were frequently made over a single 2 cm thick layer of weakly cohesive/highly porous lime mortar (Figure 2, e). Aggregate fraction is constituted of moderately sorted carbonate sands, mixed with chert and quartz, while terracotta fraction appears to be absent. This clear downgrade in the quality and durability of mosaic foundations clearly reflects a progressive loss of crafts skills and economical power of customers during Late Antiquity [23, 26]. Wall paintings Petro-mineralogical composition of wall-painting pictorial layers and tectoria has also been preliminary described elsewhere [25, 28]. Here we just recall the main features of these materials. In Ist to IVth style (II century BC to I century AD) wall-paintings, the tectorium consists of one up to two intonachino layers followed by 1 up to 4 inner arriccio and rinzaffo layers (Figure 2, g). This sequence of strata recalls Vitruvian precepts for opus albarium (VII, 3, 6). Intonachino layers are always made with a bright, highly cohesive stucco mortar [38] composed of pure lime mixed with well-sorted and perfectly mixed euhedral clasts of spathic calcite and sporadic marble fragments (Figure 3, h). Layer thicknesses range from around 0.8 cm up to 1.5 cm. Mayor modifications in the intonachino composition were highlighted in relation to Middle and Late Imperial wall-painting samples. The upper layer appears to be a unique stratum, 0.1 up to 0.2 cm thick (Figure 2, h), composed of pure lime mixed with sporadic local carbonate/silicate fluvial sands, while spathic calcite and marble fragments are totally absent. As observed in relation with mosaics, this clear modification in wall-painting tectorium composition has been connected to a progressive loss of quality and prestige of pictorial art during Late Antiquity in Aquileia [25, 28]. 675 5th Historic Mortars Conference – 19-21 June 2019 – Pamplona, Spain Conclusions This ongoing project is providing intriguing results in the field of the researches on mortarbased compounds used in antiquity. We observed a high specialization on “recipes” in relation to the function of mortars and concretes. Chronology appears to have an important role in the composition of mortar-based compounds. The analysis of the “recipes” could be pointed out as a way for dating Aquileia structures and buildings, supporting traditional dating methodologies based on stratigraphy and pottery chrono-typologies. Quarrying area are being analysed and variations in selections of raw materials will be discussed in relation with historical and economical background of Aquileia. The continue crosscheck of data obtained from such an extensive sampling is giving valuable insights for the deciphering of the relations among crafts and artisans in ancient construction and decorative activities. These considerations could be stressed as a way for renovating the discussion on the Art of Making in a crucial centre for the history of Roman Cisalpina as it was Aquileia. Author contribution Introduction: JB, GA; “State of Art” discussion: SD; Context of interest selection: SD, JB; Sampling: SD, JB; Analytical methodology: SD, MS, GA; Samples preparation and analysis: SD, MS; Data processing and interpretation: SD, JB; Conclusions: SD; Supervision: JB, GA; Writing: SD References 1. Portulano B, Urban M (2001) Materiali e tecniche murarie nel Basso e Medio Friuli in età romana. Editreg, Trieste 2. Bacchetta A (2003) Edilizia rurale romana. All’Insegna del Giglio, Firenze 3. Previato C (2015) Aquileia. Materiali, forme e sistemi costruttivi dall'età repubblicana alla tarda età imperiale. Padova University Press, Padova 4. Pizzol L (2015/2016) Archaeometric analyses of Roman Mortars in Italy: a storiographic review. MA Thesis, Sup. Prof. J Bonetto, University of Padova 5. Bugini R, Folli L (2013) Critères pour la comparaison des enduits peints romains de la Lombardie. ArcheoSciences. https://journals.openedition.org/archeosciences/3973 6. 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