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Tehnološki fakultet  Novi Sad, Univerzitet u Novom Sadu

Metodologija ispitivanja istorijskih maltera 

Manual for the Laboratory Research of Historical Mortars

Snežana Vučetić, Jonjua Ranogajec

Iz Predgovora

 

Ova knjiga je koncipirana tako da definiše osnovne termine i korake koje je neophodno sprovesti da bi se uradila kvalitetna karakterizacija istorijskih maltera. Knjiga je pre svega namenjena studentima Tehnološkog fakulteta, Katedre za inženjerstvo materijala, Arhitektonskog i Hemijskog fakulteta, ali i svim učesnicima uključenim u proces zaštite nepokretnog kulturnog nasleđa.

Knjiga je osmišljena tako da predstavlja svojevrsnu vrstu vodiča za ispitivanje istorijskih maltera od trenutka kada se istraživač nađe ispred objekta koji je predmet ispitivanja, prolazi sa njim sve faze procesa istraživanja, sve do momenta dobijanja i interpretacije rezultata. U knjizi su detaljno definisani sledeći postupci: metodologija dijagnostike stanja, in-situ ispitivanja, uzorkovanje, laboratorijska ispitivanja, interpretacije rezultata, mogućnosti korišćenja dobijenih rezultata i pregled aktuelne literature drugih istraživačkih grupa. Ovi postupci definisani su i prikazani kroz primere koji su rezultat naučnog projekta MoDeCo2000: „Dizajn maltera za konzervaciju – rimska granica na Dunavu 2000 godina kasnijeˮ (Mortar Design for Conservation – Danube Roman Frontier 2000 Years after), finansiranog kroz program PROMIS od strane Fonda za nauku Republike Srbije.

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Talanta, Volume 252, 15 January 2023, 123844

https://doi.org/10.1016/j.talanta.2022.123844

Fired pressed pellet as a sample preparation technique of choice for an energy dispersive X-ray fluorescence analysis of raw clays

Nevenka Mijatović, Milica Vasić, Ljiljana Miličić, Milena Radomirović, Zagorka Radojević

In this paper, the main subject concerns comparing different techniques to prepare raw clay samples for energy-dispersive X-ray fluorescence spectrometry (EDXRF). Three kinds of sample preparation procedures are examined, such as loose powder, pressed pellet, and fired pressed pellet. The fired pressed pellet approach was observed as a part of universal sample preparation for physic, mechanical, and instrumental analysis, which has not been previously tested as a solution in chemical analysis by the EDXRF method. The observed sample preparation techniques were compared by calculating the parameters of validation (recoveries, limit of detection - LOD, limit of quantification - LOQ, precision, and expanded uncertainties of measurements) of 11 elements (Si, Al, Fe, Ca, Mg, K, Na, Ti, P, Mn, and S) using 15 certified reference materials (CRMs). Calibration curves were created and evaluated using 30 reference materials (RM) for all three approaches. Results proved that the fired pressed pellet is the most practical and precise approach for sample preparation of raw clays.

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Materials 2023, 16(2), 642 

 https://doi.org/10.3390/ma16020642

Bio-stimulated surface healing of historical and compatible conservation mortars

The main focus of this research was the bio-stimulated healing of cracks in lime mortar samples (historical and newly designed). The investigation started from comprehensive characterisation of historical mortars, while in the next stage a compatible conservation mortar was designed and characterised, with special attention given to the contact zone formation between original and conservation mortars. The next step was the design of a bio-stimulating crack-sealing agent, a two-component liquid system: bacteria culture Sporosarcina pasteurii DSM 33 and nutrients. Both historical and conservation mortar samples were used in order to study their potentials for bio-stimulated surface-crack repair. The experiment lasted for 150 days, allowing the ureolytic bacteria Sporosarcina pasteurii DSM 33 to induce the precipitation of calcium carbonate into cracks and heal the damaged surface of the tested materials. The healing phenomenon was continuously monitored during a period of 150 days. Special attention was given to the evaluation of the morphology, chemical and structural characteristics of the deposits created in/on the surface cracks, monitored by optical microscopy, SEM, XRF and XRD analyses. The obtained results present valuable input for the application of the developed system in real environmental conditions as a solution for the future sustainable architectural conservation of traditionally prepared mortars.

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Гласник Друштва конзерватора Србије 45 (2021)

Дизајн малтера за конзервацију - Римска граница на Дунаву 2000 година касније. Научно-истраживачки пројекат MoDeCo2000 

Снежана Вучетић, Емилија Николић, Младен Јовичић, Љиљана Миличић,

Ивана Делић Николић, Хелена Хиршенбергер, Јоњауа Раногајец

Дизajн мaлтeрa зa кoнзeрвaциjу – Римскa грaницa нa Дунaву 2000 гoдинa кaсниje (Mortar Design for Conservation – Danube Roman Frontier 2000 Years After: MoDeCo2000) je нaучнoистрaживaчки прojeкaт у чиjeм су фoкусу истрaживaњa римских мaлтeрa кojи пoтичу из грaђeвинa вojних утврђeњa и нaсeљa нa подручју дунaвскoг лимeсa нa тeритoриjи дaнaшњe Рeпубликe Србиje. Нoсилaц прojeктa je Aрхeoлoшки институт (др Eмилиja Никoлић – рукoвoдилaц прojeктa и др Mлaдeн Joвичић) a спрoвoди гa зajeднo сa Teхнoлoшким фaкултeтoм Унивeрзитeтa у Нoвoм Сaду (др Снeжaнa Вучeтић и др Joњaуa Рaнoгajeц) и Институтoм зa испитивaњe мaтeриjaлa, Бeoгрaд (Љиљaнa Mиличић и Ивaнa Дeлић Никoлић). Прojeкaт трaje oд 2020. дo 2022. гoдинe и финaнсирa сe из прoгрaмa ПРOMИС, Фoндa зa нaуку Рeпубликe Србиje.

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Sustainability 2023, 15(3), 2824

https://doi.org/10.3390/su15032824

Recycling and reuse of building materials in a historical landscape -

Viminacium natural brick (Serbia)

 Emilija Nikolić, Ivana Delić-Nikolić, Mladen Jovičić, Ljiljana Miličić, Nevenka Mijatović

During the MoDeCo2000 scientific and research project on mortars used in the territory of the Roman Danube Limes in Serbia, the biggest challenge was the quest for the provenance of raw materials. The area where Viminacium, the largest city in the province of Moesia Superior developed, with millennial continuity of land use and settlement, was selected as research case study and is presented in this research. People throughout history have always used what they had at hand, and the building remains were not only reused but also recycled for new constructions. Thus, the building material of Roman Viminacium has survived in the landscape through the in situ preserved remains of Roman buildings, as well as in the structures from the later periods, up to today. To the best of our knowledge, the use of natural sediments baked during the self-combustion or combustion of underneath layers (coal in our case) for the purpose of construction was extremely rare in the Roman Empire. In this study, we follow the presence of this type of material precisely in Viminacium construction, naming it natural brick, while focusing on its potential use in lime mortars whose production was perfected in the Roman period and has never been surpassed afterward. Archaeological contexts in which this material was found have been studied, along with simultaneous work in the laboratory and in the field during the research and experimental use of the natural brick in lime mortars. We sought to determine whether this material could have been recognised by Romans in Viminacium as a potential valuable pozzolanic component of mortar, along with or instead of fired brick, being locally available and recyclable. The final confirmation of its pozzolanic features and later discussion open completely new directions for the future research of Viminacium lime mortars.

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Snežana Vučetić, Emilija Nikolić, Mladen Jovičić, Ivana Delić-Nikolić, Ljiljana Miličić, Jonjua Ranogajec, Helena Hiršenberger

Design of conservation mortars for architectural heritage is always an ambitious and inspiring task, asking for many diverse requirements to be successfully harmonised. Principally, conservation mortars need to comply with demanding chemical, mineralogical, textural, and mechanical compatibility criteria. The main aim of this paper is to show the design and development of compatible mortars for conservation of a late Roman tomb in Serbia, situated around the former Danube Limes. It is only a fragment of the MoDeCo2000 project which deals with the research of mortars from the archaeological sites along the Limes, dated to the period from the first to the sixth centuries. Laboratory activities for the sampled mortars included visual observations, stereo-optical and digital microscopy, spectrophotometry and colourimetry, mineralogical and petrographic analyses, physical–mechanical tests, thermal characterisation, mechanical and chemical separation of aggregates and binders, and characterisation of samples, binders, and aggregates using FTIR, Raman, XRF, and XRD. The obtained results enabled designing of conservation mortars mixtures based on local raw materials. Following laboratory preparation of mortar models and several cycles of mixtures optimisation, the newly developed mortars for the Roman tomb were artificially aged and compared with original samples. The models which successfully fulfilled requirements qualified for application on small test areas of the historical building, and their behaviour was closely monitored in situ. The promising research results directly led to production of compatible mortars for upcoming conservation actions on the Danube Limes in Serbia and contributed to the universal body of knowledge about Roman mortars and architecture.

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The dust that a building is transformed into when it becomes a ruin holds precious traces of the past. The hands of an archaeologist will search through it patiently, and find a necklace bead of a woman that lived in it. The hands of an architect will virtually transform the dust into a mortar, brick, or stone. The first profession sees through the unbuilt. The second one builds from it. However, both perform their work by communicating with the sciences.  Throughout history, various components were chosen, measured, and mixed into one of the most complex building composites ever - mortar, whose re-creation is of invaluable importance for architectural conservation. Geologists and chemists will best tell us about its composition. However, sometimes, while excavating a ruined wall, an archaeologist finds a mortar trowel, accidentally left by the past builder. Is this a more valuable trace for revealing the creation of a wall than the binder/aggregate ratio of the mortar used? Can we pick it up and imagine the hands that combined colourful aggregate grains with the earth, gypsum, lime, or cement?  From the exploitation, transport, and use of raw materials, to the product called mortar, we pass by the people from the past, the quarries, roads, and rivers, we look at the craftsmen working with tools, and observe the investors negotiating with engineers, and the rulers supervising the construction. The four hands from the beginning of the story can combine the chemistry of the red, blue, green, yellow, black, and white mineral grains with the found trowel, and help us revive many unknown hands from the past. Thus, the research of historic mortars for conservation purposes must not be a purely technical process. Only by understanding the multiple values of a historic building, we can adequately protect it. The project Mortar Design for Conservation – Danube Roman Frontier 2,000 Years After (MoDeCo2000), funded by the Science Fund of the Republic of Serbia, was created with the sincere intent and great hope that it could help in the future discoveries and preservation of the rich heritage in Serbia from the period of the magnificent Roman Empire, whose Danubian monuments are part of the preliminary list for UNESCO World Heritage. Different researchers and professionals - architects, archaeologists, geologists, chemists, materials scientists, physicists, biologists, restorers, craftsmen, and managers have all made an effort to get closer to the fulfillment of the wish of the project creators.  After sampling and investigating numerous mortars originating from the structures dating to the period from the 1st to the 6th century, many conclusions were made, but challenges for future researchers and conservators also arose, telling us we need to continue our work in the future, in an attempt to gain more knowledge and, thus, preserve our heritage more adequately. We welcome you to the Viminacium Archaeological Park and the 1st International Conference with Workshop, Science for Conservation of the Danube Limes. With the hope that many new fruitful collaborations between our guest researchers will be developed on this occasion, taking us one step further towards long-term technical solutions for architectural conservation and civil engineering based on nature, but also to new cognitions about the life of the past people, always for the cause of the preservation of rich world material and immaterial cultural heritage and our planet, we invite you to peruse this publication. All the authors have shown their enormous affection and passionate devotion towards the discoveries of ancient knowledge, advocating its use in the further preservation of the most monumental physical witnesses of the past – buildings, for future generations.

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PREFACE


In the summer of 2022, the 1st International Conference with Workshop - Science for Conservation of the Danube Limes was held in Viminacium, as the final event of the project Mortar Design for Conservation - Danube Roman Frontier 2000 Years After (MoDeCo2000), financed by the Science Fund of the Republic of Serbia, with the aim of gathering participants connected by a common interest - research and protection of cultural heritage. The lectures covered topics from archaeology, history of architecture and construction, geology, conservation science, archaeometry, chemistry, materials science, physical chemistry, biology, physics, history of art, practical conservation and restoration, interpretation, documentation, and protection of heritage, as well as its management. Practical work, through the building of a wall with the use of materials present in Roman Viminacium, as a unique experience, brought together a large number of participants.
Although the topic of the project was related to historical mortars, the organisers wanted to bring together researchers and experts who deal with different materials used throughout history for the construction of buildings but also for the production of artifacts. The results of extremely complex multidisciplinary studies of historical materials are important not only for gaining knowledge about their composition and methods of production, the process of exploitation of raw materials, transport, and trade, but also for all kinds of connections between people. Their use ensures responsible conservation practices with the application of materials compatible with historical ones, but also the development of new products in the field of industry. One of the project aims is the promotion of the use of local raw materials and traditional techniques in the production of conservation mortars, but also their improvement in accordance with today’s circumstances and the environment in which historical buildings are located. What all historical materials have in common is that they were mainly created using locally
available raw materials, they were guided by the experience and practicality of people, and improved
over generations.
Most of the papers in this volume of the scientific journal Archaeology and Science are dedicated to the topics of the Viminacium event, with their authors as participants. Given that the theme of the event connected an extremely large number of scientific fields, this volume includes other papers that relate to them, all contributing to the research, protection, and interpretation of cultural heritage.
Archaeology, as a humanistic science, in collaboration with natural sciences, provides solutions from the past employed by technical and technological sciences for the development of modern ones, invaluable to the contemporary world, especially regarding some of the most current topics, namely climate change and sustainable development. It is with this thought in mind that the content of this volume of the journal Archaeology and Science was conceived.

 


Emilija Nikolić
Institute of Archaeology, Belgrade

 Mladen Jovičić, Emilija Nikolić, Ivana Delić-Nikolić, Ljiljana Miličić, Snežana Vučetić, Jonjaua Ranogajec

Projekat MoDeCo2000 (Dizajn maltera za konzervaciju – Rimska granica na Dunavu 2000 godina kasnije/Mortar Design for Conservation – Danube Roman Frontier 2000 Years After: MoDeCo2000) jeste naučnoistraživački projekat finansiran iz programa PROMIS,Fonda za nauku Republike Srbije. Trajanje projekta iznosi dve godine, od sredine 2020.do sredine 2022. godine. Nosilac projekta je Arheološki institut, koga zastupaju dr Emilija Nikolić (rukovodilac) i dr Mladen Jovičić. Arheološki institut projekat sprovodi zajedno sa Institutom za ispitivanje materijala u Beogradu (Ljiljana Miličić, Ivana Delić Nikolić) i Teh-

nološkim fakultetom Univerziteta u Novom Sadu (dr Snežana Vučetić, dr Jonjaua Ranogajec). Članovi istraživačkog tima su stručnjaci različitih naučnih oblasti, kako humanističkih tako i tehničko-tehnoloških i prirodnih, te je multidisciplinarni pristup svakako jedna od najvećih vrednosti projekta.

Cilj ovog projekta je istraživanje rimskih maltera na prostoru dunavskog limesa na teritoriji današnje Republike Srbije. Istraživanje maltera doprinelo bi unapređenju naučnih saznanja o tehnikama zidanja i tehnologijama izrade maltera u rimskom periodu, kao i o građevinskim materijalima i eksploataciji sirovina. Namera je da se u okviru projekta izradibaza sa uzorcima rimskih maltera kao i baza sa saznanjima koja bi bila dobijena nakon laboratorijskih proučavanja istih. Na osnovu laboratorijskih istraživanja maltera dizajniraju se kompatibilni malteri za konzervaciju građevina koji bi bili zasnovani na upotrebi lokalnih sirovina i tradicionalnih tehnologija, odnosno donele bi se preporuke važne za konzervaciju spomenika kulture na arheološkim nalazištima u Srbiji. Sve navedeno je u bliskoj vezi saizradom nominacionog dosijea za deo međunarodnog kulturnog dobra „Granice Rimskog carstva“ pod imenom „Dunavski limes u Srbiji“, u cilju njegovog upisa na Uneskovu listu svetskog nasleđa. Nominacioni dosije izrađuju Arheološki institut i Republički zavod za zaštitu spomenika kulture.

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 Emilija Nikolić, Mladen Jovičić, Ivana Delić-Nikolić, Ljiljana Miličić, Snežana Vučetić, Jonjaua Ranogajec

The research project Mortar Design for Conservation - Danube Roman Frontier 2000 Years After (MoDeCo2000) explores Roman mortars of the former Danube Limes in Serbia. It aims to fill in some missing pieces of the puzzle about life in the Roman period in  the border territory by examining the creation of fortifications, and public and residential buildings. Finally, the project designs tailor made conservation mortar mixtures in accordance with these precious data. The project concept is based on the prevailing idea of modern architectural conservation, which requires a holistic approach, combining old building practice and new scientific knowledge about building constructions, technologies, and materials used in the Roman period in the mentioned territory, with the aim of giving science-based recommendations for future practical conservation.

Ivana Delić-Nikolić, Ljiljana Miličić, Emilija Nikolić, Mladen Jovičić, Snežana Vučetić

The research within the project Mortar Design for Conservation - Roman Danube Frontier 2000 Years After (MoDeCo2000), dealing with Roman buildings in Serbia situated along the former Danube Limes was carried out using data from archaeological, architectural, and geological contexts, combined with mineralogical, chemical and material science research. The aim of the research is to reveal unknown data on ancient provincial construction, but also to contribute to future conservation processes, offering a database of historic mortars and raw materials used at the mentioned territory during the centuries. The research has confirmed the well-known unwritten rule of using local materials in historical constructions. The unique landscape around the Viminacium Archaeological Park with the remains of structures dating to ancient, Early Byzantine, and medieval periods, is an area where four archaeological sites, with nine buildings and forty-two different mortars, were examined, making it an ideal case study for this paper.

Ljiljana Miličić, Ivana Delić-Nikolić, Emilija Nikolić, Mladen Jovičić, Snežana Vučetić

Sustainable preservation of historic buildings is a long-term process that begins with the analysis of all data related to their creation and further duration and ends with the proposal of measures to preserve their current condition and prevent future damage. In accordance with this, the most important goal of the project Mortar Design for Conservation - Danube Roman Frontier 2000 Years after - MoDeCo2000, was set. Data obtained from the archaeological, architectural, and geological context research with the thorough laboratory testing of sampled Roman mortars along the river Danube in Serbia was used to create valuable proposals for the design of compatible mortar mixtures that could be used for the conservation of the structures in the investigated area.

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Arheološki institut Beograd, Institut za ispitivanje materijala

Istorijski malteri. Od karakterizacije do konzervacije

Historical Mortars. From Characterisation to Conservation

Ivana Delić-Nikolić, Ljiljana Miličić, Emilija Nikolić

Publikacija Istorijski malteri – od karakterizacije do konzervacije predstavlja jedan od rezultata projekta Mortar Design for Conservation – Danube Roman Frontier 2000 Years After (MoDeCo2000), koji je finansirao Fond za nauku Republike Srbije od 2020. do 2022. godine kroz program PROMIS. Projekat je sproveden u saradnji Arheološkog instituta, Tehnološkog fakulteta Novi Sad Univerziteta u Novom Sadu i Instituta za ispitivanje materijala. Tema projekta su krečni malteri građevina podignutih u periodu od I do VI veka na delu dunavskog limesa koji se nalazio na teritoriji današnje Republike Srbije.

U Srbiji se nalaze ostaci brojnih građevina iz svih istorijskih perioda, ali malteri ugrađeni u njihove strukture do sada nisu bili predmet sistematskog proučavanja. Period čiji je razvoj graditeljstva najdirektnije bio uslovljen razvojem pripreme i primene krečnog maltera predstavlja vreme rimske dominacije. Kroz projekat MoDeCo2000 sprovedeno je istraživanje graditeljstva nastalog tokom ovog perioda na teritoriji dunavskog limesa – granice Rimskog carstva na reci Dunav. S obzirom na to da su rimski krečni malteri u svetu decenijama predmet brojnih naučnih projekata, MoDeCo2000 predstavlja važan doprinos naučne zajednice Republike Srbije razvoju ovih istraživanja, ne samo kroz osvetljavanje dela slike graditeljskog, pa i društveno-ekonomskog razvoja prostora centralnog Balkana u periodu od I do VI veka nove ere, već i tradicionalnog graditeljstva na predmetnoj teritoriji uopšte. Osim istraživačkog cilja projekta, kao jednako važan je bio onaj usmeren na praktičnu arhitektonsku konzervaciju, odnosno direktnu primenu naučnih rezultata projekta u procesima očuvanja istorijskih građevina u Srbiji, u skladu sa međunarodnim dokumentima iz oblasti zaštite kulturnog nasleđa.

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